# Electronic Supplementary Information for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2009
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Manfred Bochmann'
'Lewis Broomfield'
'Joseph Wright'
_publ_contact_author_name 'Manfred Bochmann'
_publ_contact_author_email M.BOCHMANN@UEA.AC.UK
_publ_section_title
;
Synthesis, Structures and Reactivity of
2-Phosphorylmethyl-1H-pyrrolato Complexes of Titanium,
Yttrium and Zinc
;
# Attachment 'Pyrrole-phosphine1.cif'
data_3a
_database_code_depnum_ccdc_archive 'CCDC 729817'
_chemical_name_common 'Compound 3a'
_chemical_melting_point ?
_chemical_formula_structural Pyr(H)-PPh2
_chemical_formula_moiety 'C17 H16 N O P'
_chemical_formula_sum 'C17 H16 N O P'
_chemical_formula_weight 281.28
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.3992(3)
_cell_length_b 5.75940(10)
_cell_length_c 22.1848(5)
_cell_angle_alpha 90.00
_cell_angle_beta 95.068(1)
_cell_angle_gamma 90.00
_cell_volume 1450.79(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 17657
_cell_measurement_theta_min 2.91
_cell_measurement_theta_max 27.48
_exptl_crystal_description slab
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.288
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 592
_exptl_absorpt_coefficient_mu 0.184
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8212
_exptl_absorpt_correction_T_max 0.9927
_exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator '10cm confocal mirrors'
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 18282
_diffrn_reflns_av_R_equivalents 0.0648
_diffrn_reflns_av_sigmaI/netI 0.0502
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 3.16
_diffrn_reflns_theta_max 27.51
_reflns_number_total 3329
_reflns_number_gt 2491
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
Structure solved in P2~1~/n as this gives best position of main residue in
cell.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+2.1072P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3329
_refine_ls_number_parameters 181
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0882
_refine_ls_R_factor_gt 0.0554
_refine_ls_wR_factor_ref 0.1174
_refine_ls_wR_factor_gt 0.1028
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_restrained_S_all 1.060
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.96440(19) 0.7090(4) 0.06001(10) 0.0251(5) Uani 1 1 d . . .
H1A H 0.9323 0.5570 0.0457 0.030 Uiso 1 1 calc R . .
H1B H 1.0201 0.7626 0.0311 0.030 Uiso 1 1 calc R . .
C2 C 1.02905(19) 0.6796(4) 0.12112(10) 0.0262(5) Uani 1 1 d . . .
C3 C 1.0861(2) 0.4918(5) 0.20661(11) 0.0376(6) Uani 1 1 d . . .
H3 H 1.0956 0.3732 0.2364 0.045 Uiso 1 1 calc R . .
C4 C 1.1353(2) 0.7075(5) 0.21087(11) 0.0385(6) Uani 1 1 d . . .
H4 H 1.1846 0.7668 0.2441 0.046 Uiso 1 1 calc R . .
C5 C 1.0994(2) 0.8265(5) 0.15665(11) 0.0343(6) Uani 1 1 d . . .
H5 H 1.1204 0.9806 0.1467 0.041 Uiso 1 1 calc R . .
C6 C 0.75182(19) 0.8090(4) 0.11650(10) 0.0257(5) Uani 1 1 d . . .
C7 C 0.7330(2) 0.9436(5) 0.16639(10) 0.0322(6) Uani 1 1 d . . .
H7 H 0.7703 1.0906 0.1716 0.039 Uiso 1 1 calc R . .
C8 C 0.6598(2) 0.8649(5) 0.20889(12) 0.0402(7) Uani 1 1 d . . .
H8 H 0.6465 0.9584 0.2429 0.048 Uiso 1 1 calc R . .
C9 C 0.6064(2) 0.6502(5) 0.20156(12) 0.0397(7) Uani 1 1 d . . .
H9 H 0.5566 0.5959 0.2307 0.048 Uiso 1 1 calc R . .
C10 C 0.6250(2) 0.5159(5) 0.15254(14) 0.0418(7) Uani 1 1 d . . .
H10 H 0.5879 0.3686 0.1477 0.050 Uiso 1 1 calc R . .
C11 C 0.6975(2) 0.5924(5) 0.10994(13) 0.0369(6) Uani 1 1 d . . .
H11 H 0.7104 0.4974 0.0761 0.044 Uiso 1 1 calc R . .
C12 C 0.7602(2) 0.8930(4) -0.01111(10) 0.0273(5) Uani 1 1 d . . .
C13 C 0.6820(3) 1.0712(5) -0.02797(13) 0.0457(7) Uani 1 1 d . . .
H13 H 0.6754 1.1999 -0.0017 0.055 Uiso 1 1 calc R . .
C14 C 0.6132(3) 1.0631(6) -0.08287(14) 0.0509(8) Uani 1 1 d . . .
H14 H 0.5590 1.1846 -0.0936 0.061 Uiso 1 1 calc R . .
C15 C 0.6234(2) 0.8812(5) -0.12149(12) 0.0398(7) Uani 1 1 d . . .
H15 H 0.5775 0.8780 -0.1594 0.048 Uiso 1 1 calc R . .
C16 C 0.7004(2) 0.7016(5) -0.10556(12) 0.0402(6) Uani 1 1 d . . .
H16 H 0.7069 0.5743 -0.1323 0.048 Uiso 1 1 calc R . .
C17 C 0.7681(2) 0.7075(5) -0.05055(11) 0.0352(6) Uani 1 1 d . . .
H17 H 0.8205 0.5832 -0.0397 0.042 Uiso 1 1 calc R . .
N1 N 1.02060(17) 0.4757(4) 0.15203(9) 0.0289(5) Uani 1 1 d . . .
H1 H 0.9796 0.3535 0.1389 0.035 Uiso 1 1 calc R . .
O1 O 0.88487(14) 1.1582(3) 0.07446(7) 0.0288(4) Uani 1 1 d . . .
P1 P 0.84529(5) 0.91552(10) 0.06122(3) 0.02400(15) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0240(11) 0.0232(12) 0.0280(12) -0.0004(10) 0.0022(9) -0.0004(9)
C2 0.0224(11) 0.0273(12) 0.0287(12) 0.0009(10) 0.0017(9) -0.0017(9)
C3 0.0348(14) 0.0496(17) 0.0275(13) 0.0059(12) -0.0020(10) -0.0022(12)
C4 0.0344(14) 0.0478(17) 0.0318(14) -0.0045(12) -0.0059(11) -0.0070(12)
C5 0.0310(13) 0.0311(14) 0.0398(14) -0.0009(11) -0.0028(11) -0.0058(11)
C6 0.0231(11) 0.0239(12) 0.0300(12) 0.0025(10) 0.0019(9) 0.0035(9)
C7 0.0343(13) 0.0335(15) 0.0286(12) -0.0020(11) 0.0023(10) -0.0035(11)
C8 0.0397(15) 0.0518(19) 0.0297(13) -0.0010(12) 0.0068(11) 0.0014(13)
C9 0.0300(13) 0.0475(18) 0.0428(15) 0.0156(13) 0.0100(11) 0.0038(12)
C10 0.0308(14) 0.0286(14) 0.0673(19) 0.0074(14) 0.0119(13) -0.0023(11)
C11 0.0341(13) 0.0272(13) 0.0507(16) -0.0030(12) 0.0101(11) -0.0018(11)
C12 0.0276(12) 0.0270(12) 0.0269(11) 0.0020(10) 0.0014(9) -0.0029(10)
C13 0.0575(18) 0.0332(15) 0.0433(15) -0.0065(13) -0.0133(13) 0.0131(14)
C14 0.0506(18) 0.0469(18) 0.0510(17) 0.0013(15) -0.0195(14) 0.0118(15)
C15 0.0360(14) 0.0513(18) 0.0302(13) 0.0054(12) -0.0074(11) -0.0112(13)
C16 0.0423(15) 0.0463(17) 0.0311(14) -0.0062(12) -0.0020(11) -0.0026(13)
C17 0.0378(14) 0.0345(15) 0.0324(13) -0.0032(11) -0.0020(11) 0.0027(11)
N1 0.0280(10) 0.0282(11) 0.0298(10) 0.0001(8) -0.0008(8) -0.0065(8)
O1 0.0307(9) 0.0223(9) 0.0330(9) -0.0008(7) 0.0013(7) -0.0034(7)
P1 0.0246(3) 0.0211(3) 0.0260(3) -0.0006(3) 0.0007(2) -0.0011(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.494(3) . ?
C1 P1 1.807(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.367(3) . ?
C2 N1 1.368(3) . ?
C3 C4 1.363(4) . ?
C3 N1 1.368(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.413(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.384(3) . ?
C6 C11 1.394(3) . ?
C6 P1 1.802(2) . ?
C7 C8 1.389(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.366(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.389(3) . ?
C12 C13 1.389(3) . ?
C12 P1 1.805(2) . ?
C13 C14 1.390(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.365(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N1 H1 0.8800 . ?
O1 P1 1.4900(17) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 111.85(16) . . ?
C2 C1 H1A 109.2 . . ?
P1 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
P1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C5 C2 N1 107.8(2) . . ?
C5 C2 C1 132.1(2) . . ?
N1 C2 C1 120.1(2) . . ?
C4 C3 N1 108.2(2) . . ?
C4 C3 H3 125.9 . . ?
N1 C3 H3 125.9 . . ?
C3 C4 C5 107.3(2) . . ?
C3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
C2 C5 C4 107.5(2) . . ?
C2 C5 H5 126.2 . . ?
C4 C5 H5 126.2 . . ?
C7 C6 C11 119.1(2) . . ?
C7 C6 P1 119.76(19) . . ?
C11 C6 P1 121.17(19) . . ?
C6 C7 C8 120.3(2) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C6 120.1(3) . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
C17 C12 C13 118.3(2) . . ?
C17 C12 P1 123.78(19) . . ?
C13 C12 P1 117.90(19) . . ?
C12 C13 C14 120.7(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.1(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 119.9(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C12 120.8(3) . . ?
C16 C17 H17 119.6 . . ?
C12 C17 H17 119.6 . . ?
C2 N1 C3 109.2(2) . . ?
C2 N1 H1 125.4 . . ?
C3 N1 H1 125.4 . . ?
O1 P1 C6 111.85(11) . . ?
O1 P1 C12 111.86(11) . . ?
C6 P1 C12 106.08(11) . . ?
O1 P1 C1 113.93(10) . . ?
C6 P1 C1 106.03(11) . . ?
C12 P1 C1 106.56(11) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C5 -67.6(3) . . . . ?
P1 C1 C2 N1 110.8(2) . . . . ?
N1 C3 C4 C5 -0.6(3) . . . . ?
N1 C2 C5 C4 0.2(3) . . . . ?
C1 C2 C5 C4 178.8(2) . . . . ?
C3 C4 C5 C2 0.2(3) . . . . ?
C11 C6 C7 C8 -0.8(4) . . . . ?
P1 C6 C7 C8 179.10(19) . . . . ?
C6 C7 C8 C9 0.6(4) . . . . ?
C7 C8 C9 C10 -0.3(4) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C9 C10 C11 C6 -0.4(4) . . . . ?
C7 C6 C11 C10 0.7(4) . . . . ?
P1 C6 C11 C10 -179.2(2) . . . . ?
C17 C12 C13 C14 0.2(4) . . . . ?
P1 C12 C13 C14 -179.5(2) . . . . ?
C12 C13 C14 C15 -1.2(5) . . . . ?
C13 C14 C15 C16 1.4(5) . . . . ?
C14 C15 C16 C17 -0.6(4) . . . . ?
C15 C16 C17 C12 -0.4(4) . . . . ?
C13 C12 C17 C16 0.6(4) . . . . ?
P1 C12 C17 C16 -179.8(2) . . . . ?
C5 C2 N1 C3 -0.6(3) . . . . ?
C1 C2 N1 C3 -179.4(2) . . . . ?
C4 C3 N1 C2 0.7(3) . . . . ?
C7 C6 P1 O1 -5.0(2) . . . . ?
C11 C6 P1 O1 174.83(19) . . . . ?
C7 C6 P1 C12 -127.25(19) . . . . ?
C11 C6 P1 C12 52.6(2) . . . . ?
C7 C6 P1 C1 119.71(19) . . . . ?
C11 C6 P1 C1 -60.4(2) . . . . ?
C17 C12 P1 O1 141.5(2) . . . . ?
C13 C12 P1 O1 -38.9(2) . . . . ?
C17 C12 P1 C6 -96.3(2) . . . . ?
C13 C12 P1 C6 83.3(2) . . . . ?
C17 C12 P1 C1 16.4(2) . . . . ?
C13 C12 P1 C1 -164.0(2) . . . . ?
C2 C1 P1 O1 66.37(19) . . . . ?
C2 C1 P1 C6 -57.08(19) . . . . ?
C2 C1 P1 C12 -169.78(16) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.88 2.05 2.868(3) 154.3 1_545
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 27.51
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.358
_refine_diff_density_min -0.249
_refine_diff_density_rms 0.061
#==END
data_5a
_database_code_depnum_ccdc_archive 'CCDC 729818'
_chemical_name_common 'Compound 5a'
_chemical_melting_point ?
_chemical_formula_structural '[Pyr-P(O)Ph2]2Ti(NMe2)2'
_chemical_formula_moiety 'C38 H42 N4 O2 P2 Ti'
_chemical_formula_sum 'C38 H42 N4 O2 P2 Ti'
_chemical_formula_weight 696.60
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P b c n'
_symmetry_space_group_name_Hall '-P 2n 2ab'
_symmetry_Int_Tables_number 60
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
_cell_length_a 15.392(5)
_cell_length_b 12.636(5)
_cell_length_c 18.352(5)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 3569(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 59850
_cell_measurement_theta_min 2.91
_cell_measurement_theta_max 27.48
_exptl_crystal_description plate
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.296
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1464
_exptl_absorpt_coefficient_mu 0.368
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.844
_exptl_absorpt_correction_T_max 0.996
_exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method '\f & \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 32736
_diffrn_reflns_av_R_equivalents 0.1723
_diffrn_reflns_av_sigmaI/netI 0.1199
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 3.66
_diffrn_reflns_theta_max 27.55
_reflns_number_total 4102
_reflns_number_gt 2222
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.0380P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4102
_refine_ls_number_parameters 215
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1938
_refine_ls_R_factor_gt 0.0957
_refine_ls_wR_factor_ref 0.1825
_refine_ls_wR_factor_gt 0.1467
_refine_ls_goodness_of_fit_ref 1.125
_refine_ls_restrained_S_all 1.125
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.0000 0.13943(10) 0.2500 0.0265(3) Uani 1 2 d S . .
N1 N -0.1369(3) 0.1157(3) 0.2657(2) 0.0290(10) Uani 1 1 d . . .
N2 N -0.0048(3) 0.2413(3) 0.1730(3) 0.0365(12) Uani 1 1 d . . .
O1 O -0.0110(2) 0.0153(3) 0.17275(18) 0.0279(8) Uani 1 1 d . . .
P1 P -0.08431(9) -0.05954(11) 0.15384(8) 0.0257(3) Uani 1 1 d . . .
C1 C -0.1524(3) -0.0766(4) 0.2326(3) 0.0289(12) Uani 1 1 d . . .
H1A H -0.1998 -0.1243 0.2209 0.035 Uiso 1 1 calc R . .
H1B H -0.1189 -0.1078 0.2719 0.035 Uiso 1 1 calc R . .
C2 C -0.1882(3) 0.0277(4) 0.2565(3) 0.0264(11) Uani 1 1 d . . .
C3 C -0.1931(3) 0.1968(4) 0.2847(3) 0.0299(13) Uani 1 1 d . . .
H3 H -0.1763 0.2660 0.2948 0.036 Uiso 1 1 calc R . .
C4 C -0.2774(4) 0.1602(5) 0.2864(3) 0.0338(13) Uani 1 1 d . . .
H4 H -0.3267 0.1994 0.2978 0.041 Uiso 1 1 calc R . .
C5 C -0.2748(3) 0.0530(5) 0.2677(3) 0.0330(13) Uani 1 1 d . . .
H5 H -0.3220 0.0075 0.2636 0.040 Uiso 1 1 calc R . .
C6 C -0.0417(3) -0.1864(4) 0.1269(3) 0.0280(12) Uani 1 1 d . . .
C7 C -0.0907(4) -0.2787(5) 0.1356(3) 0.0368(14) Uani 1 1 d . . .
H7 H -0.1457 -0.2755 0.1564 0.044 Uiso 1 1 calc R . .
C8 C -0.0567(4) -0.3755(5) 0.1128(4) 0.0455(16) Uani 1 1 d . . .
H8 H -0.0890 -0.4372 0.1183 0.055 Uiso 1 1 calc R . .
C9 C 0.0248(4) -0.3793(5) 0.0822(3) 0.0402(15) Uani 1 1 d . . .
H9 H 0.0475 -0.4440 0.0672 0.048 Uiso 1 1 calc R . .
C10 C 0.0730(4) -0.2889(5) 0.0733(3) 0.0356(14) Uani 1 1 d . . .
H10 H 0.1281 -0.2924 0.0526 0.043 Uiso 1 1 calc R . .
C11 C 0.0394(4) -0.1920(5) 0.0954(3) 0.0324(13) Uani 1 1 d . . .
H11 H 0.0718 -0.1306 0.0889 0.039 Uiso 1 1 calc R . .
C12 C -0.1495(3) -0.0107(4) 0.0793(3) 0.0286(12) Uani 1 1 d . . .
C13 C -0.1636(3) -0.0708(5) 0.0168(3) 0.0329(13) Uani 1 1 d . . .
H13 H -0.1397 -0.1382 0.0133 0.039 Uiso 1 1 calc R . .
C14 C -0.2130(4) -0.0311(5) -0.0404(3) 0.0419(16) Uani 1 1 d . . .
H14 H -0.2230 -0.0723 -0.0816 0.050 Uiso 1 1 calc R . .
C15 C -0.2474(4) 0.0702(5) -0.0360(3) 0.0433(16) Uani 1 1 d . . .
H15 H -0.2797 0.0977 -0.0745 0.052 Uiso 1 1 calc R . .
C16 C -0.2335(4) 0.1297(5) 0.0259(3) 0.0403(15) Uani 1 1 d . . .
H16 H -0.2575 0.1971 0.0292 0.048 Uiso 1 1 calc R . .
C17 C -0.1847(4) 0.0911(5) 0.0828(3) 0.0361(14) Uani 1 1 d . . .
H17 H -0.1750 0.1329 0.1237 0.043 Uiso 1 1 calc R . .
C18 C 0.0294(4) 0.2215(5) 0.1009(3) 0.0475(17) Uani 1 1 d . . .
H18A H 0.0658 0.2795 0.0864 0.071 Uiso 1 1 calc R . .
H18B H -0.0178 0.2146 0.0670 0.071 Uiso 1 1 calc R . .
H18C H 0.0628 0.1574 0.1013 0.071 Uiso 1 1 calc R . .
C19 C -0.0517(5) 0.3425(6) 0.1726(5) 0.083(3) Uani 1 1 d . . .
H19A H -0.0999 0.3382 0.1395 0.125 Uiso 1 1 calc R . .
H19B H -0.0132 0.3980 0.1573 0.125 Uiso 1 1 calc R . .
H19C H -0.0728 0.3575 0.2207 0.125 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0290(7) 0.0207(7) 0.0298(8) 0.000 0.0005(6) 0.000
N1 0.028(2) 0.029(2) 0.030(3) -0.002(2) 0.0002(19) 0.0011(19)
N2 0.039(3) 0.029(2) 0.042(3) 0.013(2) 0.007(2) 0.006(2)
O1 0.033(2) 0.0258(19) 0.025(2) 0.0008(15) 0.0006(16) -0.0006(16)
P1 0.0274(7) 0.0245(7) 0.0253(7) -0.0011(6) -0.0008(6) 0.0004(6)
C1 0.028(3) 0.029(3) 0.030(3) 0.002(2) -0.003(2) 0.000(2)
C2 0.030(3) 0.032(3) 0.017(3) 0.003(2) 0.000(2) 0.001(2)
C3 0.034(3) 0.029(3) 0.026(3) 0.001(2) -0.003(2) 0.010(2)
C4 0.032(3) 0.041(4) 0.029(3) 0.001(3) 0.000(2) 0.009(3)
C5 0.030(3) 0.042(3) 0.028(3) -0.001(3) -0.001(2) 0.000(3)
C6 0.028(3) 0.031(3) 0.025(3) -0.002(2) -0.004(2) 0.000(2)
C7 0.032(3) 0.038(3) 0.040(4) 0.000(3) 0.006(3) 0.002(3)
C8 0.051(4) 0.030(3) 0.055(4) -0.001(3) -0.002(3) 0.000(3)
C9 0.051(4) 0.028(3) 0.041(4) 0.000(3) 0.001(3) 0.012(3)
C10 0.031(3) 0.044(4) 0.033(3) 0.003(3) 0.003(3) 0.010(3)
C11 0.037(3) 0.035(3) 0.025(3) -0.001(3) -0.005(3) 0.001(3)
C12 0.022(3) 0.037(3) 0.026(3) 0.006(3) -0.001(2) 0.001(2)
C13 0.035(3) 0.032(3) 0.032(3) 0.001(3) 0.001(3) -0.001(2)
C14 0.046(4) 0.053(4) 0.026(3) -0.001(3) -0.007(3) -0.010(3)
C15 0.031(3) 0.057(4) 0.041(4) 0.009(3) -0.010(3) 0.002(3)
C16 0.039(3) 0.040(4) 0.041(4) 0.009(3) 0.006(3) 0.016(3)
C17 0.037(3) 0.036(3) 0.036(3) 0.004(3) -0.002(3) 0.009(3)
C18 0.046(4) 0.061(4) 0.036(4) 0.011(3) 0.002(3) -0.004(3)
C19 0.090(6) 0.050(5) 0.109(7) 0.038(5) 0.052(5) 0.030(4)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N2 1.913(4) 4 ?
Ti1 N2 1.913(4) . ?
Ti1 O1 2.121(4) . ?
Ti1 O1 2.121(4) 4 ?
Ti1 N1 2.147(4) 4 ?
Ti1 N1 2.147(4) . ?
N1 C2 1.375(6) . ?
N1 C3 1.385(6) . ?
N2 C18 1.447(7) . ?
N2 C19 1.469(8) . ?
O1 P1 1.513(4) . ?
P1 C1 1.798(5) . ?
P1 C6 1.801(5) . ?
P1 C12 1.805(5) . ?
C1 C2 1.494(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C5 1.386(7) . ?
C3 C4 1.378(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C11 1.378(7) . ?
C6 C7 1.397(8) . ?
C7 C8 1.395(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.376(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.389(8) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.393(8) . ?
C12 C17 1.397(7) . ?
C13 C14 1.391(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ti1 N2 95.4(3) 4 . ?
N2 Ti1 O1 173.98(18) 4 . ?
N2 Ti1 O1 90.05(17) . . ?
N2 Ti1 O1 90.05(17) 4 4 ?
N2 Ti1 O1 173.98(18) . 4 ?
O1 Ti1 O1 84.64(19) . 4 ?
N2 Ti1 N1 98.91(19) 4 4 ?
N2 Ti1 N1 91.89(18) . 4 ?
O1 Ti1 N1 83.44(15) . 4 ?
O1 Ti1 N1 84.72(15) 4 4 ?
N2 Ti1 N1 91.89(18) 4 . ?
N2 Ti1 N1 98.91(19) . . ?
O1 Ti1 N1 84.72(15) . . ?
O1 Ti1 N1 83.44(15) 4 . ?
N1 Ti1 N1 164.0(2) 4 . ?
C2 N1 C3 105.7(4) . . ?
C2 N1 Ti1 131.3(3) . . ?
C3 N1 Ti1 122.9(4) . . ?
C18 N2 C19 108.9(5) . . ?
C18 N2 Ti1 123.1(4) . . ?
C19 N2 Ti1 127.5(4) . . ?
P1 O1 Ti1 132.5(2) . . ?
O1 P1 C1 109.0(2) . . ?
O1 P1 C6 110.4(2) . . ?
C1 P1 C6 109.0(3) . . ?
O1 P1 C12 112.0(2) . . ?
C1 P1 C12 109.0(2) . . ?
C6 P1 C12 107.4(3) . . ?
C2 C1 P1 110.2(4) . . ?
C2 C1 H1A 109.6 . . ?
P1 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
P1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C5 110.3(5) . . ?
N1 C2 C1 122.6(4) . . ?
C5 C2 C1 127.0(5) . . ?
C4 C3 N1 110.2(5) . . ?
C4 C3 H3 124.9 . . ?
N1 C3 H3 124.9 . . ?
C3 C4 C5 107.0(5) . . ?
C3 C4 H4 126.5 . . ?
C5 C4 H4 126.5 . . ?
C2 C5 C4 106.8(5) . . ?
C2 C5 H5 126.6 . . ?
C4 C5 H5 126.6 . . ?
C11 C6 C7 119.6(5) . . ?
C11 C6 P1 119.4(4) . . ?
C7 C6 P1 121.0(4) . . ?
C8 C7 C6 119.7(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C9 C8 C7 119.7(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.9(6) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.8(5) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C6 C11 C10 120.4(6) . . ?
C6 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C17 118.7(5) . . ?
C13 C12 P1 121.6(4) . . ?
C17 C12 P1 119.7(4) . . ?
C14 C13 C12 120.7(6) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 119.5(6) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 121.1(6) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C12 120.2(6) . . ?
C16 C17 H17 119.9 . . ?
C12 C17 H17 119.9 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ti1 N1 C2 -147.9(5) 4 . . . ?
N2 Ti1 N1 C2 116.4(5) . . . . ?
O1 Ti1 N1 C2 27.2(5) . . . . ?
O1 Ti1 N1 C2 -58.0(5) 4 . . . ?
N1 Ti1 N1 C2 -15.4(4) 4 . . . ?
N2 Ti1 N1 C3 36.2(4) 4 . . . ?
N2 Ti1 N1 C3 -59.6(4) . . . . ?
O1 Ti1 N1 C3 -148.8(4) . . . . ?
O1 Ti1 N1 C3 126.0(4) 4 . . . ?
N1 Ti1 N1 C3 168.6(4) 4 . . . ?
N2 Ti1 N2 C18 150.6(5) 4 . . . ?
N1 Ti1 N2 C18 51.5(5) 4 . . . ?
N1 Ti1 N2 C18 -116.6(5) . . . . ?
N2 Ti1 N2 C19 -38.2(6) 4 . . . ?
O1 Ti1 N2 C19 139.2(6) . . . . ?
N1 Ti1 N2 C19 -137.4(6) 4 . . . ?
N1 Ti1 N2 C19 54.5(6) . . . . ?
N2 Ti1 O1 P1 -107.5(3) . . . . ?
O1 Ti1 O1 P1 75.3(3) 4 . . . ?
N1 Ti1 O1 P1 160.6(3) 4 . . . ?
N1 Ti1 O1 P1 -8.6(3) . . . . ?
Ti1 O1 P1 C1 -26.9(4) . . . . ?
Ti1 O1 P1 C6 -146.6(3) . . . . ?
Ti1 O1 P1 C12 93.8(3) . . . . ?
O1 P1 C1 C2 59.1(4) . . . . ?
C6 P1 C1 C2 179.6(4) . . . . ?
C12 P1 C1 C2 -63.5(4) . . . . ?
C3 N1 C2 C5 1.4(6) . . . . ?
Ti1 N1 C2 C5 -175.1(4) . . . . ?
C3 N1 C2 C1 177.5(5) . . . . ?
Ti1 N1 C2 C1 1.0(8) . . . . ?
P1 C1 C2 N1 -49.0(6) . . . . ?
P1 C1 C2 C5 126.4(5) . . . . ?
C2 N1 C3 C4 -0.7(6) . . . . ?
Ti1 N1 C3 C4 176.2(4) . . . . ?
N1 C3 C4 C5 -0.2(6) . . . . ?
N1 C2 C5 C4 -1.5(6) . . . . ?
C1 C2 C5 C4 -177.4(5) . . . . ?
C3 C4 C5 C2 1.0(6) . . . . ?
O1 P1 C6 C11 -28.5(5) . . . . ?
C1 P1 C6 C11 -148.2(4) . . . . ?
C12 P1 C6 C11 93.9(4) . . . . ?
O1 P1 C6 C7 153.5(4) . . . . ?
C1 P1 C6 C7 33.8(5) . . . . ?
C12 P1 C6 C7 -84.2(5) . . . . ?
C11 C6 C7 C8 0.6(8) . . . . ?
P1 C6 C7 C8 178.6(5) . . . . ?
C6 C7 C8 C9 0.1(9) . . . . ?
C7 C8 C9 C10 -0.3(9) . . . . ?
C8 C9 C10 C11 -0.1(9) . . . . ?
C7 C6 C11 C10 -1.0(8) . . . . ?
P1 C6 C11 C10 -179.1(4) . . . . ?
C9 C10 C11 C6 0.8(8) . . . . ?
O1 P1 C12 C13 124.7(4) . . . . ?
C1 P1 C12 C13 -114.6(5) . . . . ?
C6 P1 C12 C13 3.4(5) . . . . ?
O1 P1 C12 C17 -53.1(5) . . . . ?
C1 P1 C12 C17 67.6(5) . . . . ?
C6 P1 C12 C17 -174.5(4) . . . . ?
C17 C12 C13 C14 -1.2(8) . . . . ?
P1 C12 C13 C14 -179.1(4) . . . . ?
C12 C13 C14 C15 1.2(9) . . . . ?
C13 C14 C15 C16 -1.2(9) . . . . ?
C14 C15 C16 C17 1.2(9) . . . . ?
C15 C16 C17 C12 -1.2(9) . . . . ?
C13 C12 C17 C16 1.2(8) . . . . ?
P1 C12 C17 C16 179.1(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 27.55
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.457
_refine_diff_density_min -0.461
_refine_diff_density_rms 0.105
# ==END
data_5c
_database_code_depnum_ccdc_archive 'CCDC 729819'
_chemical_name_common 'Compound 5c'
_chemical_melting_point ?
_chemical_formula_structural '[3-(t-Bu)-Pyr-P(O)Ph2]2Ti(NMe2)2.(2.5PhH)'
_chemical_formula_moiety 'C46 H58 N4 O2 P2 Ti, 2.5(C6 H6)'
_chemical_formula_sum 'C61 H73 N4 O2 P2 Ti'
_chemical_formula_weight 1004.07
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.1366(13)
_cell_length_b 16.2331(17)
_cell_length_c 16.3753(17)
_cell_angle_alpha 108.236(9)
_cell_angle_beta 95.852(9)
_cell_angle_gamma 107.144(9)
_cell_volume 2860.2(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 140(2)
_cell_measurement_reflns_used 4523
_cell_measurement_theta_min 3.3565
_cell_measurement_theta_max 33.9468
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.30
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.166
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1070
_exptl_absorpt_coefficient_mu 0.250
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.467
_exptl_absorpt_correction_T_max 0.930
_exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 140(2)
_diffrn_radiation_probe x-ray
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method 'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 29354
_diffrn_reflns_av_R_equivalents 0.1019
_diffrn_reflns_av_sigmaI/netI 0.2230
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.36
_diffrn_reflns_theta_max 25.00
_reflns_number_total 9990
_reflns_number_gt 3928
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution 'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
One molecule of toluene was only very poorly ordered, and was therefore
refined usin isotropic thermal parameters only.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9990
_refine_ls_number_parameters 584
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1815
_refine_ls_R_factor_gt 0.0811
_refine_ls_wR_factor_ref 0.2274
_refine_ls_wR_factor_gt 0.1901
_refine_ls_goodness_of_fit_ref 0.877
_refine_ls_restrained_S_all 0.877
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.60092(9) 0.27374(7) 0.13806(6) 0.0330(3) Uani 1 1 d . . .
C1 C 0.7536(5) 0.4248(4) 0.0313(3) 0.0358(14) Uani 1 1 d . . .
H1A H 0.7067 0.4618 0.0557 0.043 Uiso 1 1 calc R . .
H1B H 0.8012 0.4547 -0.0024 0.043 Uiso 1 1 calc R . .
C2 C 0.6735(4) 0.3302(4) -0.0281(4) 0.0290(13) Uani 1 1 d . . .
C3 C 0.5495(5) 0.1879(4) -0.0678(4) 0.0370(14) Uani 1 1 d . . .
H3 H 0.4981 0.1337 -0.0657 0.044 Uiso 1 1 calc R . .
C4 C 0.5772(5) 0.1989(4) -0.1450(4) 0.0334(14) Uani 1 1 d . . .
C5 C 0.6591(5) 0.2909(4) -0.1171(4) 0.0354(14) Uani 1 1 d . . .
H5 H 0.6963 0.3191 -0.1532 0.042 Uiso 1 1 calc R . .
C6 C 0.5335(6) 0.1303(4) -0.2375(4) 0.0458(16) Uani 1 1 d . . .
C7 C 0.4415(6) 0.0422(4) -0.2431(4) 0.0562(18) Uani 1 1 d . . .
H7A H 0.3729 0.0548 -0.2264 0.084 Uiso 1 1 calc R . .
H7B H 0.4724 0.0170 -0.2042 0.084 Uiso 1 1 calc R . .
H7C H 0.4203 -0.0014 -0.3024 0.084 Uiso 1 1 calc R . .
C8 C 0.4770(10) 0.1709(5) -0.2960(5) 0.117(4) Uani 1 1 d . . .
H8A H 0.4438 0.1250 -0.3540 0.176 Uiso 1 1 calc R . .
H8B H 0.5360 0.2235 -0.2993 0.176 Uiso 1 1 calc R . .
H8C H 0.4159 0.1895 -0.2714 0.176 Uiso 1 1 calc R . .
C9 C 0.6332(7) 0.1047(6) -0.2732(6) 0.119(4) Uani 1 1 d . . .
H9A H 0.6791 0.0926 -0.2300 0.178 Uiso 1 1 calc R . .
H9B H 0.6825 0.1548 -0.2868 0.178 Uiso 1 1 calc R . .
H9C H 0.6016 0.0504 -0.3257 0.178 Uiso 1 1 calc R . .
C10 C 0.9454(4) 0.5315(4) 0.1885(4) 0.0348(14) Uani 1 1 d . . .
C11 C 0.9703(5) 0.5545(4) 0.2784(4) 0.0375(14) Uani 1 1 d . . .
H11 H 0.9384 0.5097 0.3019 0.045 Uiso 1 1 calc R . .
C12 C 1.0407(5) 0.6411(5) 0.3340(4) 0.0492(17) Uani 1 1 d . . .
H12 H 1.0568 0.6548 0.3945 0.059 Uiso 1 1 calc R . .
C13 C 1.0881(5) 0.7088(4) 0.2994(5) 0.0515(17) Uani 1 1 d . . .
H13 H 1.1355 0.7682 0.3365 0.062 Uiso 1 1 calc R . .
C14 C 1.0641(5) 0.6868(4) 0.2100(5) 0.0496(17) Uani 1 1 d . . .
H14 H 1.0966 0.7319 0.1871 0.060 Uiso 1 1 calc R . .
C15 C 0.9942(5) 0.6009(4) 0.1536(4) 0.0405(15) Uani 1 1 d . . .
H15 H 0.9786 0.5878 0.0932 0.049 Uiso 1 1 calc R . .
C16 C 0.9352(5) 0.3533(4) 0.0679(3) 0.0345(14) Uani 1 1 d . . .
C17 C 0.8807(6) 0.2599(4) 0.0186(4) 0.0479(16) Uani 1 1 d . . .
H17 H 0.7997 0.2321 0.0110 0.057 Uiso 1 1 calc R . .
C18 C 0.9478(6) 0.2071(5) -0.0200(4) 0.0533(18) Uani 1 1 d . . .
H18 H 0.9107 0.1446 -0.0534 0.064 Uiso 1 1 calc R . .
C19 C 1.0678(7) 0.2471(6) -0.0088(4) 0.064(2) Uani 1 1 d . . .
H19 H 1.1116 0.2117 -0.0343 0.076 Uiso 1 1 calc R . .
C20 C 1.1230(6) 0.3400(5) 0.0404(5) 0.0595(19) Uani 1 1 d . . .
H20 H 1.2040 0.3673 0.0474 0.071 Uiso 1 1 calc R . .
C21 C 1.0577(5) 0.3926(4) 0.0793(4) 0.0444(16) Uani 1 1 d . . .
H21 H 1.0958 0.4548 0.1134 0.053 Uiso 1 1 calc R . .
C22 C 0.6554(5) 0.4905(4) 0.3158(3) 0.0353(14) Uani 1 1 d . . .
H22A H 0.7354 0.5026 0.3064 0.042 Uiso 1 1 calc R . .
H22B H 0.6545 0.5428 0.3644 0.042 Uiso 1 1 calc R . .
C23 C 0.6161(5) 0.4046(4) 0.3369(3) 0.0311(13) Uani 1 1 d . . .
C24 C 0.5617(5) 0.2573(4) 0.3179(4) 0.0431(16) Uani 1 1 d . . .
H24 H 0.5447 0.1939 0.2924 0.052 Uiso 1 1 calc R . .
C25 C 0.5482(5) 0.2998(4) 0.3997(4) 0.0448(16) Uani 1 1 d . . .
C26 C 0.5825(5) 0.3947(4) 0.4120(4) 0.0435(16) Uani 1 1 d . . .
H26 H 0.5824 0.4419 0.4619 0.052 Uiso 1 1 calc R . .
C27 C 0.5102(7) 0.2558(5) 0.4664(4) 0.063(2) Uani 1 1 d . . .
C28 C 0.4514(8) 0.3094(5) 0.5285(5) 0.089(3) Uani 1 1 d . . .
H28A H 0.5044 0.3719 0.5584 0.133 Uiso 1 1 calc R . .
H28B H 0.4311 0.2811 0.5709 0.133 Uiso 1 1 calc R . .
H28C H 0.3811 0.3095 0.4959 0.133 Uiso 1 1 calc R . .
C29 C 0.4314(9) 0.1569(5) 0.4230(5) 0.102(3) Uani 1 1 d . . .
H29A H 0.4119 0.1311 0.4671 0.153 Uiso 1 1 calc R . .
H29B H 0.4715 0.1228 0.3858 0.153 Uiso 1 1 calc R . .
H29C H 0.3605 0.1534 0.3882 0.153 Uiso 1 1 calc R . .
C30 C 0.6254(8) 0.2607(7) 0.5237(6) 0.107(3) Uani 1 1 d . . .
H30A H 0.6792 0.3233 0.5478 0.160 Uiso 1 1 calc R . .
H30B H 0.6617 0.2220 0.4877 0.160 Uiso 1 1 calc R . .
H30C H 0.6056 0.2396 0.5708 0.160 Uiso 1 1 calc R . .
C31 C 0.6117(5) 0.5741(4) 0.1890(4) 0.0334(14) Uani 1 1 d . . .
C32 C 0.5483(5) 0.5781(4) 0.1148(4) 0.0407(15) Uani 1 1 d . . .
H32 H 0.4776 0.5307 0.0835 0.049 Uiso 1 1 calc R . .
C33 C 0.5900(5) 0.6522(4) 0.0875(4) 0.0415(15) Uani 1 1 d . . .
H33 H 0.5470 0.6546 0.0385 0.050 Uiso 1 1 calc R . .
C34 C 0.6963(6) 0.7228(4) 0.1335(4) 0.0518(17) Uani 1 1 d . . .
H34 H 0.7246 0.7727 0.1157 0.062 Uiso 1 1 calc R . .
C35 C 0.7594(6) 0.7181(4) 0.2058(4) 0.0525(18) Uani 1 1 d . . .
H35 H 0.8309 0.7649 0.2361 0.063 Uiso 1 1 calc R . .
C36 C 0.7183(5) 0.6452(4) 0.2341(4) 0.0460(16) Uani 1 1 d . . .
H36 H 0.7618 0.6435 0.2833 0.055 Uiso 1 1 calc R . .
C37 C 0.4152(5) 0.4672(4) 0.2450(4) 0.0371(14) Uani 1 1 d . . .
C38 C 0.3523(5) 0.3886(5) 0.2602(4) 0.0535(18) Uani 1 1 d . . .
H38 H 0.3819 0.3408 0.2544 0.064 Uiso 1 1 calc R . .
C39 C 0.2448(6) 0.3828(5) 0.2842(4) 0.0614(19) Uani 1 1 d . . .
H39 H 0.2026 0.3309 0.2952 0.074 Uiso 1 1 calc R . .
C40 C 0.1997(6) 0.4528(6) 0.2919(4) 0.065(2) Uani 1 1 d . . .
H40 H 0.1278 0.4482 0.3087 0.078 Uiso 1 1 calc R . .
C41 C 0.2608(6) 0.5298(5) 0.2746(4) 0.0538(18) Uani 1 1 d . . .
H41 H 0.2290 0.5761 0.2782 0.065 Uiso 1 1 calc R . .
C42 C 0.3690(5) 0.5381(4) 0.2521(3) 0.0398(15) Uani 1 1 d . . .
H42 H 0.4110 0.5905 0.2417 0.048 Uiso 1 1 calc R . .
C43 C 0.3948(5) 0.1042(4) 0.1211(4) 0.0425(15) Uani 1 1 d . . .
H43A H 0.3513 0.1160 0.1666 0.064 Uiso 1 1 calc R . .
H43B H 0.4581 0.0860 0.1404 0.064 Uiso 1 1 calc R . .
H43C H 0.3432 0.0557 0.0690 0.064 Uiso 1 1 calc R . .
C44 C 0.3454(5) 0.2059(4) 0.0585(4) 0.0455(16) Uani 1 1 d . . .
H44A H 0.3085 0.1566 0.0028 0.068 Uiso 1 1 calc R . .
H44B H 0.3754 0.2633 0.0495 0.068 Uiso 1 1 calc R . .
H44C H 0.2886 0.2093 0.0950 0.068 Uiso 1 1 calc R . .
C45 C 0.7769(5) 0.2094(4) 0.2152(4) 0.0515(17) Uani 1 1 d . . .
H45A H 0.7616 0.1637 0.2422 0.077 Uiso 1 1 calc R . .
H45B H 0.7901 0.2690 0.2587 0.077 Uiso 1 1 calc R . .
H45C H 0.8457 0.2109 0.1907 0.077 Uiso 1 1 calc R . .
C46 C 0.6527(5) 0.0966(4) 0.0767(4) 0.0422(15) Uani 1 1 d . . .
H46A H 0.7208 0.0980 0.0514 0.063 Uiso 1 1 calc R . .
H46B H 0.5858 0.0831 0.0318 0.063 Uiso 1 1 calc R . .
H46C H 0.6369 0.0496 0.1022 0.063 Uiso 1 1 calc R . .
N1 N 0.6076(4) 0.2676(3) 0.0060(3) 0.0310(11) Uani 1 1 d . . .
N2 N 0.6037(4) 0.3189(3) 0.2765(3) 0.0380(12) Uani 1 1 d . . .
N3 N 0.4431(4) 0.1880(3) 0.1019(3) 0.0344(11) Uani 1 1 d . . .
N4 N 0.6746(4) 0.1862(3) 0.1448(3) 0.0347(11) Uani 1 1 d . . .
O1 O 0.7753(3) 0.3748(2) 0.1737(2) 0.0336(9) Uani 1 1 d . . .
O2 O 0.5491(3) 0.3891(2) 0.1446(2) 0.0324(9) Uani 1 1 d . . .
P1 P 0.84824(13) 0.41858(10) 0.11903(10) 0.0341(4) Uani 1 1 d . . .
P2 P 0.55776(13) 0.47510(10) 0.21866(10) 0.0331(4) Uani 1 1 d . . .
C47 C 0.0083(8) 0.5870(6) 0.5514(5) 0.077(2) Uani 1 1 d . . .
H47 H 0.0123 0.6459 0.5860 0.092 Uiso 1 1 calc R . .
C48 C 0.1093(7) 0.5662(6) 0.5481(5) 0.067(2) Uani 1 1 d . . .
H48 H 0.1824 0.6098 0.5800 0.080 Uiso 1 1 calc R . .
C49 C -0.0991(7) 0.5219(7) 0.5044(5) 0.074(2) Uani 1 1 d . . .
H49 H -0.1667 0.5376 0.5079 0.089 Uiso 1 1 calc R . .
C50 C 1.0487(10) 0.0067(9) 0.2649(6) 0.290(12) Uani 1 1 d G . .
H50 H 1.0811 -0.0036 0.3131 0.349 Uiso 1 1 calc R . .
C51 C 1.1220(6) 0.0534(9) 0.2217(7) 0.264(11) Uani 1 1 d G . .
H51 H 1.2035 0.0742 0.2410 0.317 Uiso 1 1 calc R . .
C52 C 1.0735(7) 0.0688(6) 0.1497(7) 0.188(6) Uani 1 1 d G . .
H52 H 1.1226 0.1000 0.1208 0.225 Uiso 1 1 calc R . .
C53 C 0.9517(7) 0.0377(6) 0.1208(5) 0.126(4) Uani 1 1 d G . .
H53 H 0.9193 0.0480 0.0726 0.152 Uiso 1 1 calc R . .
C54 C 0.8784(5) -0.0090(5) 0.1640(6) 0.100(3) Uani 1 1 d G . .
H54 H 0.7969 -0.0298 0.1447 0.120 Uiso 1 1 calc R . .
C55 C 0.9268(9) -0.0244(6) 0.2361(6) 0.191(6) Uani 1 1 d G . .
H55 H 0.8778 -0.0556 0.2650 0.229 Uiso 1 1 calc R . .
C56 C 0.8888(12) 0.0598(7) 0.5443(8) 0.330(11) Uiso 1 1 d G . .
H56 H 0.8477 0.0185 0.5686 0.396 Uiso 1 1 calc R . .
C57 C 1.0108(12) 0.1005(8) 0.5709(6) 0.263(8) Uiso 1 1 d G . .
H57 H 1.0515 0.0865 0.6130 0.315 Uiso 1 1 calc R . .
C58 C 1.0722(7) 0.1622(7) 0.5347(7) 0.161(5) Uiso 1 1 d G . .
H58 H 1.1539 0.1894 0.5525 0.194 Uiso 1 1 calc R . .
C59 C 1.0115(10) 0.1831(6) 0.4718(7) 0.289(9) Uiso 1 1 d G . .
H59 H 1.0525 0.2244 0.4475 0.346 Uiso 1 1 calc R . .
C60 C 0.8894(10) 0.1424(8) 0.4451(6) 0.173(5) Uiso 1 1 d G . .
H60 H 0.8488 0.1564 0.4030 0.207 Uiso 1 1 calc R . .
C61 C 0.8281(7) 0.0807(7) 0.4814(8) 0.218(6) Uiso 1 1 d G . .
H61 H 0.7464 0.0535 0.4636 0.261 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0322(6) 0.0395(6) 0.0360(6) 0.0195(5) 0.0201(5) 0.0142(5)
C1 0.047(4) 0.040(4) 0.037(3) 0.023(3) 0.030(3) 0.023(3)
C2 0.026(3) 0.033(3) 0.035(4) 0.019(3) 0.016(3) 0.009(3)
C3 0.041(4) 0.031(3) 0.040(4) 0.015(3) 0.014(3) 0.010(3)
C4 0.033(3) 0.039(4) 0.035(4) 0.015(3) 0.016(3) 0.016(3)
C5 0.032(3) 0.043(4) 0.043(4) 0.024(3) 0.022(3) 0.015(3)
C6 0.057(4) 0.050(4) 0.032(4) 0.017(3) 0.021(3) 0.016(3)
C7 0.056(4) 0.062(4) 0.044(4) 0.021(3) 0.021(3) 0.005(4)
C8 0.231(12) 0.080(6) 0.038(5) 0.030(4) 0.004(6) 0.049(7)
C9 0.051(5) 0.102(7) 0.120(7) -0.050(6) 0.046(5) -0.005(5)
C10 0.021(3) 0.055(4) 0.037(4) 0.018(3) 0.017(3) 0.020(3)
C11 0.023(3) 0.048(4) 0.044(4) 0.019(3) 0.015(3) 0.011(3)
C12 0.030(4) 0.071(5) 0.044(4) 0.021(4) 0.005(3) 0.014(4)
C13 0.034(4) 0.045(4) 0.065(5) 0.016(4) 0.011(3) 0.003(3)
C14 0.039(4) 0.051(4) 0.061(5) 0.029(4) 0.018(3) 0.007(3)
C15 0.036(4) 0.045(4) 0.037(4) 0.015(3) 0.007(3) 0.009(3)
C16 0.039(4) 0.046(4) 0.027(3) 0.021(3) 0.018(3) 0.016(3)
C17 0.044(4) 0.057(4) 0.055(4) 0.025(4) 0.027(3) 0.025(4)
C18 0.060(5) 0.058(4) 0.063(5) 0.029(4) 0.024(4) 0.038(4)
C19 0.060(5) 0.094(6) 0.062(5) 0.032(5) 0.028(4) 0.054(5)
C20 0.032(4) 0.087(6) 0.073(5) 0.032(5) 0.023(4) 0.031(4)
C21 0.032(4) 0.062(4) 0.042(4) 0.018(3) 0.006(3) 0.022(3)
C22 0.035(3) 0.035(3) 0.040(4) 0.011(3) 0.021(3) 0.016(3)
C23 0.029(3) 0.034(3) 0.029(3) 0.007(3) 0.013(3) 0.011(3)
C24 0.060(4) 0.036(4) 0.036(4) 0.017(3) 0.021(3) 0.013(3)
C25 0.053(4) 0.041(4) 0.038(4) 0.013(3) 0.016(3) 0.011(3)
C26 0.042(4) 0.053(4) 0.031(4) 0.008(3) 0.014(3) 0.016(3)
C27 0.091(6) 0.066(5) 0.039(4) 0.019(4) 0.034(4) 0.030(4)
C28 0.111(7) 0.093(6) 0.066(5) 0.040(5) 0.048(5) 0.019(5)
C29 0.162(9) 0.061(5) 0.072(6) 0.027(4) 0.061(6) 0.009(6)
C30 0.110(7) 0.169(9) 0.102(7) 0.092(7) 0.044(6) 0.081(7)
C31 0.034(4) 0.045(4) 0.030(3) 0.014(3) 0.018(3) 0.022(3)
C32 0.032(4) 0.040(4) 0.049(4) 0.016(3) 0.014(3) 0.009(3)
C33 0.036(4) 0.062(4) 0.039(4) 0.025(3) 0.014(3) 0.026(3)
C34 0.050(4) 0.065(5) 0.052(4) 0.034(4) 0.014(4) 0.020(4)
C35 0.045(4) 0.044(4) 0.060(5) 0.022(4) 0.007(4) 0.002(3)
C36 0.040(4) 0.046(4) 0.048(4) 0.023(3) 0.005(3) 0.005(3)
C37 0.030(3) 0.051(4) 0.039(4) 0.019(3) 0.012(3) 0.022(3)
C38 0.042(4) 0.089(5) 0.056(4) 0.043(4) 0.027(3) 0.036(4)
C39 0.041(4) 0.079(5) 0.073(5) 0.042(4) 0.028(4) 0.011(4)
C40 0.048(4) 0.105(6) 0.074(5) 0.050(5) 0.041(4) 0.041(5)
C41 0.048(4) 0.074(5) 0.052(4) 0.020(4) 0.020(3) 0.038(4)
C42 0.028(3) 0.056(4) 0.034(4) 0.015(3) 0.011(3) 0.012(3)
C43 0.044(4) 0.042(4) 0.047(4) 0.022(3) 0.021(3) 0.013(3)
C44 0.039(4) 0.049(4) 0.048(4) 0.020(3) 0.017(3) 0.009(3)
C45 0.053(4) 0.057(4) 0.055(4) 0.030(3) 0.018(4) 0.021(3)
C46 0.033(4) 0.044(4) 0.055(4) 0.021(3) 0.022(3) 0.012(3)
N1 0.033(3) 0.035(3) 0.033(3) 0.016(2) 0.021(2) 0.015(2)
N2 0.040(3) 0.049(3) 0.038(3) 0.026(3) 0.018(2) 0.019(2)
N3 0.031(3) 0.042(3) 0.038(3) 0.020(2) 0.016(2) 0.016(2)
N4 0.033(3) 0.035(3) 0.037(3) 0.014(2) 0.015(2) 0.010(2)
O1 0.031(2) 0.042(2) 0.035(2) 0.0240(18) 0.0107(18) 0.0095(18)
O2 0.028(2) 0.037(2) 0.038(2) 0.0212(19) 0.0155(17) 0.0098(17)
P1 0.0290(9) 0.0434(10) 0.0377(9) 0.0202(8) 0.0168(7) 0.0142(7)
P2 0.0267(9) 0.0388(9) 0.0391(10) 0.0179(8) 0.0149(7) 0.0122(7)
C47 0.064(6) 0.116(7) 0.058(5) 0.037(5) 0.009(5) 0.037(6)
C48 0.049(5) 0.106(7) 0.055(5) 0.046(5) 0.015(4) 0.022(5)
C49 0.048(6) 0.110(7) 0.063(5) 0.030(5) 0.012(4) 0.028(5)
C50 0.088(11) 0.62(4) 0.236(18) 0.25(2) 0.065(12) 0.117(18)
C51 0.069(9) 0.57(3) 0.130(12) 0.112(16) 0.044(8) 0.092(14)
C52 0.085(10) 0.303(18) 0.240(17) 0.172(15) 0.090(10) 0.062(11)
C53 0.084(8) 0.196(11) 0.173(10) 0.118(9) 0.075(8) 0.082(8)
C54 0.091(7) 0.084(6) 0.128(9) 0.030(6) 0.043(7) 0.039(6)
C55 0.121(12) 0.263(16) 0.154(13) 0.087(12) 0.008(10) 0.013(11)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N3 1.907(4) . ?
Ti1 N4 1.913(4) . ?
Ti1 O2 2.120(3) . ?
Ti1 N1 2.144(4) . ?
Ti1 N2 2.146(5) . ?
Ti1 O1 2.148(3) . ?
C1 C2 1.497(7) . ?
C1 P1 1.794(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C5 1.365(7) . ?
C2 N1 1.397(6) . ?
C3 C4 1.392(7) . ?
C3 N1 1.393(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.426(7) . ?
C4 C6 1.499(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.502(8) . ?
C6 C9 1.506(9) . ?
C6 C8 1.532(9) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.378(7) . ?
C10 C15 1.422(7) . ?
C10 P1 1.787(6) . ?
C11 C12 1.367(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.371(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.361(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.387(7) . ?
C16 C21 1.401(8) . ?
C16 P1 1.795(6) . ?
C17 C18 1.404(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.374(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.387(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.495(7) . ?
C22 P2 1.786(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C26 1.376(7) . ?
C23 N2 1.385(6) . ?
C24 C25 1.353(8) . ?
C24 N2 1.384(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.413(7) . ?
C25 C27 1.520(8) . ?
C26 H26 0.9300 . ?
C27 C29 1.496(9) . ?
C27 C28 1.503(10) . ?
C27 C30 1.570(10) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C36 1.394(7) . ?
C31 C32 1.400(7) . ?
C31 P2 1.783(6) . ?
C32 C33 1.388(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.391(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.377(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.382(7) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.391(8) . ?
C37 C42 1.402(7) . ?
C37 P2 1.803(6) . ?
C38 C39 1.386(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.378(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.382(9) . ?
C40 H40 0.9300 . ?
C41 C42 1.379(8) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 N3 1.458(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 N3 1.467(6) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 N4 1.474(7) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 N4 1.458(6) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
O1 P1 1.510(3) . ?
O2 P2 1.503(4) . ?
C47 C48 1.367(10) . ?
C47 C49 1.372(10) . ?
C47 H47 0.9300 . ?
C48 C49 1.379(10) 2_566 ?
C48 H48 0.9300 . ?
C49 C48 1.379(10) 2_566 ?
C49 H49 0.9300 . ?
C50 C51 1.3900 . ?
C50 C55 1.3900 . ?
C50 H50 0.9300 . ?
C51 C52 1.3900 . ?
C51 H51 0.9300 . ?
C52 C53 1.3900 . ?
C52 H52 0.9300 . ?
C53 C54 1.3900 . ?
C53 H53 0.9300 . ?
C54 C55 1.3900 . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
C56 C57 1.3900 . ?
C56 C61 1.3900 . ?
C56 H56 0.9300 . ?
C57 C58 1.3900 . ?
C57 H57 0.9300 . ?
C58 C59 1.3900 . ?
C58 H58 0.9300 . ?
C59 C60 1.3900 . ?
C59 H59 0.9300 . ?
C60 C61 1.3900 . ?
C60 H60 0.9300 . ?
C61 H61 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ti1 N4 95.88(19) . . ?
N3 Ti1 O2 94.11(16) . . ?
N4 Ti1 O2 169.56(17) . . ?
N3 Ti1 N1 91.92(17) . . ?
N4 Ti1 N1 100.20(18) . . ?
O2 Ti1 N1 82.44(14) . . ?
N3 Ti1 N2 96.07(18) . . ?
N4 Ti1 N2 92.30(18) . . ?
O2 Ti1 N2 83.63(15) . . ?
N1 Ti1 N2 164.40(17) . . ?
N3 Ti1 O1 176.36(16) . . ?
N4 Ti1 O1 87.13(16) . . ?
O2 Ti1 O1 83.00(13) . . ?
N1 Ti1 O1 85.53(15) . . ?
N2 Ti1 O1 85.83(15) . . ?
C2 C1 P1 110.7(3) . . ?
C2 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C5 C2 N1 111.2(5) . . ?
C5 C2 C1 127.7(5) . . ?
N1 C2 C1 121.0(5) . . ?
C4 C3 N1 112.2(5) . . ?
C4 C3 H3 123.9 . . ?
N1 C3 H3 123.9 . . ?
C3 C4 C5 104.6(5) . . ?
C3 C4 C6 128.7(5) . . ?
C5 C4 C6 126.7(5) . . ?
C2 C5 C4 108.0(5) . . ?
C2 C5 H5 126.0 . . ?
C4 C5 H5 126.0 . . ?
C4 C6 C7 112.1(5) . . ?
C4 C6 C9 110.6(5) . . ?
C7 C6 C9 106.9(6) . . ?
C4 C6 C8 109.8(5) . . ?
C7 C6 C8 107.3(6) . . ?
C9 C6 C8 110.0(7) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 118.4(5) . . ?
C11 C10 P1 120.0(4) . . ?
C15 C10 P1 121.5(4) . . ?
C12 C11 C10 121.8(6) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C13 119.4(6) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 119.3(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C15 C14 C13 122.1(6) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C14 C15 C10 119.0(6) . . ?
C14 C15 H15 120.5 . . ?
C10 C15 H15 120.5 . . ?
C17 C16 C21 118.5(5) . . ?
C17 C16 P1 119.3(4) . . ?
C21 C16 P1 122.2(5) . . ?
C16 C17 C18 120.1(6) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.6(6) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.9(6) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C21 120.0(6) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C16 120.9(6) . . ?
C20 C21 H21 119.5 . . ?
C16 C21 H21 119.5 . . ?
C23 C22 P2 108.8(4) . . ?
C23 C22 H22A 109.9 . . ?
P2 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
P2 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C26 C23 N2 109.7(5) . . ?
C26 C23 C22 128.6(5) . . ?
N2 C23 C22 121.7(5) . . ?
C25 C24 N2 112.4(5) . . ?
C25 C24 H24 123.8 . . ?
N2 C24 H24 123.8 . . ?
C24 C25 C26 105.4(5) . . ?
C24 C25 C27 127.5(6) . . ?
C26 C25 C27 127.0(5) . . ?
C23 C26 C25 107.8(5) . . ?
C23 C26 H26 126.1 . . ?
C25 C26 H26 126.1 . . ?
C29 C27 C28 110.3(7) . . ?
C29 C27 C25 112.0(5) . . ?
C28 C27 C25 111.7(6) . . ?
C29 C27 C30 109.0(7) . . ?
C28 C27 C30 106.6(6) . . ?
C25 C27 C30 107.1(6) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 118.8(5) . . ?
C36 C31 P2 122.2(4) . . ?
C32 C31 P2 118.9(4) . . ?
C33 C32 C31 120.6(5) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.9(5) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 119.4(6) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 121.2(6) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C35 C36 C31 120.1(6) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C38 C37 C42 120.2(5) . . ?
C38 C37 P2 117.9(4) . . ?
C42 C37 P2 121.9(5) . . ?
C39 C38 C37 118.9(6) . . ?
C39 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
C40 C39 C38 120.9(6) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 120.2(6) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C42 C41 C40 120.1(6) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C37 119.7(6) . . ?
C41 C42 H42 120.2 . . ?
C37 C42 H42 120.2 . . ?
N3 C43 H43A 109.5 . . ?
N3 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N3 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N3 C44 H44A 109.5 . . ?
N3 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N3 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N4 C45 H45A 109.5 . . ?
N4 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N4 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N4 C46 H46A 109.5 . . ?
N4 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N4 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C3 N1 C2 104.0(4) . . ?
C3 N1 Ti1 123.2(3) . . ?
C2 N1 Ti1 132.4(4) . . ?
C24 N2 C23 104.7(4) . . ?
C24 N2 Ti1 122.1(4) . . ?
C23 N2 Ti1 131.5(3) . . ?
C43 N3 C44 108.6(4) . . ?
C43 N3 Ti1 128.5(4) . . ?
C44 N3 Ti1 122.4(3) . . ?
C46 N4 C45 111.1(4) . . ?
C46 N4 Ti1 126.0(4) . . ?
C45 N4 Ti1 122.2(3) . . ?
P1 O1 Ti1 130.7(2) . . ?
P2 O2 Ti1 133.6(2) . . ?
O1 P1 C10 108.8(2) . . ?
O1 P1 C1 110.1(2) . . ?
C10 P1 C1 110.5(2) . . ?
O1 P1 C16 112.7(2) . . ?
C10 P1 C16 108.5(3) . . ?
C1 P1 C16 106.2(2) . . ?
O2 P2 C31 110.3(2) . . ?
O2 P2 C22 110.8(2) . . ?
C31 P2 C22 108.6(3) . . ?
O2 P2 C37 110.5(2) . . ?
C31 P2 C37 109.1(3) . . ?
C22 P2 C37 107.5(3) . . ?
C48 C47 C49 120.7(8) . . ?
C48 C47 H47 119.7 . . ?
C49 C47 H47 119.7 . . ?
C47 C48 C49 117.6(8) . 2_566 ?
C47 C48 H48 121.2 . . ?
C49 C48 H48 121.2 2_566 . ?
C47 C49 C48 121.7(8) . 2_566 ?
C47 C49 H49 119.2 . . ?
C48 C49 H49 119.2 2_566 . ?
C51 C50 C55 120.0 . . ?
C51 C50 H50 120.0 . . ?
C55 C50 H50 120.0 . . ?
C52 C51 C50 120.0 . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 120.0 . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C54 C55 C50 120.0 . . ?
C54 C55 H55 120.0 . . ?
C50 C55 H55 120.0 . . ?
C57 C56 C61 120.0 . . ?
C57 C56 H56 120.0 . . ?
C61 C56 H56 120.0 . . ?
C56 C57 C58 120.0 . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 C59 120.0 . . ?
C57 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
C60 C59 C58 120.0 . . ?
C60 C59 H59 120.0 . . ?
C58 C59 H59 120.0 . . ?
C59 C60 C61 120.0 . . ?
C59 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
C60 C61 C56 120.0 . . ?
C60 C61 H61 120.0 . . ?
C56 C61 H61 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C5 -125.5(5) . . . . ?
P1 C1 C2 N1 50.0(6) . . . . ?
N1 C3 C4 C5 0.9(6) . . . . ?
N1 C3 C4 C6 -179.9(5) . . . . ?
N1 C2 C5 C4 2.0(6) . . . . ?
C1 C2 C5 C4 177.9(5) . . . . ?
C3 C4 C5 C2 -1.7(6) . . . . ?
C6 C4 C5 C2 179.0(5) . . . . ?
C3 C4 C6 C7 4.8(8) . . . . ?
C5 C4 C6 C7 -176.2(5) . . . . ?
C3 C4 C6 C9 -114.4(7) . . . . ?
C5 C4 C6 C9 64.6(8) . . . . ?
C3 C4 C6 C8 123.9(7) . . . . ?
C5 C4 C6 C8 -57.0(8) . . . . ?
C15 C10 C11 C12 -0.5(8) . . . . ?
P1 C10 C11 C12 -177.5(4) . . . . ?
C10 C11 C12 C13 0.5(9) . . . . ?
C11 C12 C13 C14 -0.6(9) . . . . ?
C12 C13 C14 C15 0.6(9) . . . . ?
C13 C14 C15 C10 -0.6(9) . . . . ?
C11 C10 C15 C14 0.5(8) . . . . ?
P1 C10 C15 C14 177.5(4) . . . . ?
C21 C16 C17 C18 -1.1(8) . . . . ?
P1 C16 C17 C18 -178.3(4) . . . . ?
C16 C17 C18 C19 0.5(9) . . . . ?
C17 C18 C19 C20 -0.3(10) . . . . ?
C18 C19 C20 C21 0.8(10) . . . . ?
C19 C20 C21 C16 -1.5(9) . . . . ?
C17 C16 C21 C20 1.6(8) . . . . ?
P1 C16 C21 C20 178.7(4) . . . . ?
P2 C22 C23 C26 -120.6(6) . . . . ?
P2 C22 C23 N2 56.3(6) . . . . ?
N2 C24 C25 C26 0.5(7) . . . . ?
N2 C24 C25 C27 -176.6(6) . . . . ?
N2 C23 C26 C25 0.4(6) . . . . ?
C22 C23 C26 C25 177.5(5) . . . . ?
C24 C25 C26 C23 -0.5(7) . . . . ?
C27 C25 C26 C23 176.6(6) . . . . ?
C24 C25 C27 C29 -29.0(10) . . . . ?
C26 C25 C27 C29 154.4(7) . . . . ?
C24 C25 C27 C28 -153.2(7) . . . . ?
C26 C25 C27 C28 30.2(10) . . . . ?
C24 C25 C27 C30 90.4(8) . . . . ?
C26 C25 C27 C30 -86.1(8) . . . . ?
C36 C31 C32 C33 -1.0(8) . . . . ?
P2 C31 C32 C33 -177.3(4) . . . . ?
C31 C32 C33 C34 0.7(8) . . . . ?
C32 C33 C34 C35 0.2(9) . . . . ?
C33 C34 C35 C36 -0.8(10) . . . . ?
C34 C35 C36 C31 0.5(10) . . . . ?
C32 C31 C36 C35 0.4(8) . . . . ?
P2 C31 C36 C35 176.6(5) . . . . ?
C42 C37 C38 C39 -1.3(9) . . . . ?
P2 C37 C38 C39 177.3(5) . . . . ?
C37 C38 C39 C40 0.8(10) . . . . ?
C38 C39 C40 C41 0.7(11) . . . . ?
C39 C40 C41 C42 -1.9(10) . . . . ?
C40 C41 C42 C37 1.4(9) . . . . ?
C38 C37 C42 C41 0.2(8) . . . . ?
P2 C37 C42 C41 -178.3(4) . . . . ?
C4 C3 N1 C2 0.3(6) . . . . ?
C4 C3 N1 Ti1 -173.8(3) . . . . ?
C5 C2 N1 C3 -1.4(6) . . . . ?
C1 C2 N1 C3 -177.6(4) . . . . ?
C5 C2 N1 Ti1 171.9(4) . . . . ?
C1 C2 N1 Ti1 -4.2(7) . . . . ?
N3 Ti1 N1 C3 -33.5(4) . . . . ?
N4 Ti1 N1 C3 62.8(4) . . . . ?
O2 Ti1 N1 C3 -127.4(4) . . . . ?
N2 Ti1 N1 C3 -154.4(6) . . . . ?
O1 Ti1 N1 C3 149.1(4) . . . . ?
N3 Ti1 N1 C2 154.2(4) . . . . ?
N4 Ti1 N1 C2 -109.5(4) . . . . ?
O2 Ti1 N1 C2 60.3(4) . . . . ?
N2 Ti1 N1 C2 33.3(9) . . . . ?
O1 Ti1 N1 C2 -23.2(4) . . . . ?
C25 C24 N2 C23 -0.3(7) . . . . ?
C25 C24 N2 Ti1 -166.8(4) . . . . ?
C26 C23 N2 C24 -0.1(6) . . . . ?
C22 C23 N2 C24 -177.5(5) . . . . ?
C26 C23 N2 Ti1 164.6(4) . . . . ?
C22 C23 N2 Ti1 -12.8(7) . . . . ?
N3 Ti1 N2 C24 45.7(4) . . . . ?
N4 Ti1 N2 C24 -50.5(4) . . . . ?
O2 Ti1 N2 C24 139.2(4) . . . . ?
N1 Ti1 N2 C24 166.1(6) . . . . ?
O1 Ti1 N2 C24 -137.4(4) . . . . ?
N3 Ti1 N2 C23 -116.8(5) . . . . ?
N4 Ti1 N2 C23 147.0(5) . . . . ?
O2 Ti1 N2 C23 -23.3(5) . . . . ?
N1 Ti1 N2 C23 3.6(9) . . . . ?
O1 Ti1 N2 C23 60.1(5) . . . . ?
N4 Ti1 N3 C43 29.0(5) . . . . ?
O2 Ti1 N3 C43 -148.0(4) . . . . ?
N1 Ti1 N3 C43 129.5(4) . . . . ?
N2 Ti1 N3 C43 -63.9(5) . . . . ?
N4 Ti1 N3 C44 -160.1(4) . . . . ?
O2 Ti1 N3 C44 22.9(4) . . . . ?
N1 Ti1 N3 C44 -59.6(4) . . . . ?
N2 Ti1 N3 C44 106.9(4) . . . . ?
N3 Ti1 N4 C46 49.9(4) . . . . ?
O2 Ti1 N4 C46 -147.0(8) . . . . ?
N1 Ti1 N4 C46 -43.1(4) . . . . ?
N2 Ti1 N4 C46 146.2(4) . . . . ?
O1 Ti1 N4 C46 -128.1(4) . . . . ?
N3 Ti1 N4 C45 -141.0(4) . . . . ?
O2 Ti1 N4 C45 22.2(12) . . . . ?
N1 Ti1 N4 C45 126.0(4) . . . . ?
N2 Ti1 N4 C45 -44.6(4) . . . . ?
O1 Ti1 N4 C45 41.1(4) . . . . ?
N4 Ti1 O1 P1 105.4(3) . . . . ?
O2 Ti1 O1 P1 -78.0(3) . . . . ?
N1 Ti1 O1 P1 4.9(3) . . . . ?
N2 Ti1 O1 P1 -162.1(3) . . . . ?
N3 Ti1 O2 P2 114.6(3) . . . . ?
N4 Ti1 O2 P2 -48.6(11) . . . . ?
N1 Ti1 O2 P2 -154.1(3) . . . . ?
N2 Ti1 O2 P2 18.9(3) . . . . ?
O1 Ti1 O2 P2 -67.7(3) . . . . ?
Ti1 O1 P1 C10 151.2(3) . . . . ?
Ti1 O1 P1 C1 29.9(4) . . . . ?
Ti1 O1 P1 C16 -88.5(3) . . . . ?
C11 C10 P1 O1 19.1(5) . . . . ?
C15 C10 P1 O1 -157.8(4) . . . . ?
C11 C10 P1 C1 140.1(4) . . . . ?
C15 C10 P1 C1 -36.8(5) . . . . ?
C11 C10 P1 C16 -103.8(4) . . . . ?
C15 C10 P1 C16 79.2(5) . . . . ?
C2 C1 P1 O1 -60.8(4) . . . . ?
C2 C1 P1 C10 178.9(4) . . . . ?
C2 C1 P1 C16 61.5(4) . . . . ?
C17 C16 P1 O1 52.1(5) . . . . ?
C21 C16 P1 O1 -124.9(4) . . . . ?
C17 C16 P1 C10 172.7(4) . . . . ?
C21 C16 P1 C10 -4.4(5) . . . . ?
C17 C16 P1 C1 -68.5(5) . . . . ?
C21 C16 P1 C1 114.4(5) . . . . ?
Ti1 O2 P2 C31 133.6(3) . . . . ?
Ti1 O2 P2 C22 13.3(4) . . . . ?
Ti1 O2 P2 C37 -105.7(3) . . . . ?
C36 C31 P2 O2 -117.1(5) . . . . ?
C32 C31 P2 O2 59.1(5) . . . . ?
C36 C31 P2 C22 4.5(5) . . . . ?
C32 C31 P2 C22 -179.3(4) . . . . ?
C36 C31 P2 C37 121.3(5) . . . . ?
C32 C31 P2 C37 -62.5(5) . . . . ?
C23 C22 P2 O2 -54.2(4) . . . . ?
C23 C22 P2 C31 -175.5(4) . . . . ?
C23 C22 P2 C37 66.5(4) . . . . ?
C38 C37 P2 O2 51.4(5) . . . . ?
C42 C37 P2 O2 -130.0(4) . . . . ?
C38 C37 P2 C31 172.9(4) . . . . ?
C42 C37 P2 C31 -8.5(6) . . . . ?
C38 C37 P2 C22 -69.5(5) . . . . ?
C42 C37 P2 C22 109.0(5) . . . . ?
C49 C47 C48 C49 0.3(12) . . . 2_566 ?
C48 C47 C49 C48 -0.3(12) . . . 2_566 ?
C55 C50 C51 C52 0.0 . . . . ?
C50 C51 C52 C53 0.0 . . . . ?
C51 C52 C53 C54 0.0 . . . . ?
C52 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 C50 0.0 . . . . ?
C51 C50 C55 C54 0.0 . . . . ?
C61 C56 C57 C58 0.0 . . . . ?
C56 C57 C58 C59 0.0 . . . . ?
C57 C58 C59 C60 0.0 . . . . ?
C58 C59 C60 C61 0.0 . . . . ?
C59 C60 C61 C56 0.0 . . . . ?
C57 C56 C61 C60 0.0 . . . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 0.644
_refine_diff_density_min -0.523
_refine_diff_density_rms 0.090
#==END
data_5d
_database_code_depnum_ccdc_archive 'CCDC 729820'
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_structural '[Pyr-P(O)Cy2]2Ti(NMe2)2'
_chemical_formula_moiety 'C38 H66 N4 O2 P2 Ti'
_chemical_formula_sum 'C38 H66 N4 O2 P2 Ti'
_chemical_formula_weight 720.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.7254(5)
_cell_length_b 19.2509(7)
_cell_length_c 19.6142(8)
_cell_angle_alpha 81.173(3)
_cell_angle_beta 88.666(2)
_cell_angle_gamma 89.788(3)
_cell_volume 4000.8(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 128503
_cell_measurement_theta_min 2.91
_cell_measurement_theta_max 27.48
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.197
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1560
_exptl_absorpt_coefficient_mu 0.330
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6427
_exptl_absorpt_correction_T_max 0.9837
_exptl_absorpt_process_details '(SADABS 2007/2; Sheldrick, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method '\f & \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 44782
_diffrn_reflns_av_R_equivalents 0.0865
_diffrn_reflns_av_sigmaI/netI 0.0744
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 2.94
_diffrn_reflns_theta_max 22.50
_reflns_number_total 10375
_reflns_number_gt 8151
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The crystal showed evidence of twinning. This could be partially resolved
using the instructions:
TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 4
BASF 0.09987 0.20000 0.09667
in the .ins file. Unresolved twinning gave left several significant Q-peaks.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1658P)^2^+36.7696P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10375
_refine_ls_number_parameters 858
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1541
_refine_ls_R_factor_gt 0.1244
_refine_ls_wR_factor_ref 0.3343
_refine_ls_wR_factor_gt 0.3093
_refine_ls_goodness_of_fit_ref 1.067
_refine_ls_restrained_S_all 1.067
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 1.05897(19) 0.01121(9) 0.24605(10) 0.0288(5) Uani 1 1 d . . .
N1 N 0.9519(9) -0.0482(4) 0.3314(4) 0.031(2) Uani 1 1 d . . .
N2 N 1.0680(9) -0.0749(4) 0.1930(4) 0.030(2) Uani 1 1 d . . .
N3 N 1.1459(10) 0.0694(5) 0.1704(5) 0.038(2) Uani 1 1 d . . .
N4 N 1.2054(10) -0.0070(5) 0.3022(5) 0.042(2) Uani 1 1 d . . .
O1 O 1.0064(7) 0.1003(4) 0.2834(3) 0.0317(18) Uani 1 1 d . . .
O2 O 0.8762(7) 0.0277(4) 0.2028(4) 0.0362(19) Uani 1 1 d . . .
P1 P 0.9391(3) 0.11193(14) 0.35027(14) 0.0289(7) Uani 1 1 d . . .
P2 P 0.8216(3) 0.00165(15) 0.14301(15) 0.0360(8) Uani 1 1 d . . .
C1 C 0.9632(13) 0.0369(5) 0.4161(6) 0.041(3) Uani 1 1 d . . .
H1A H 1.0533 0.0318 0.4257 0.049 Uiso 1 1 calc R . .
H1B H 0.9189 0.0443 0.4592 0.049 Uiso 1 1 calc R . .
C2 C 0.9166(11) -0.0282(6) 0.3936(6) 0.036(3) Uani 1 1 d . . .
C3 C 0.8899(13) -0.1111(6) 0.3297(6) 0.046(3) Uani 1 1 d . . .
H3 H 0.8977 -0.1381 0.2931 0.055 Uiso 1 1 calc R . .
C4 C 0.8166(14) -0.1289(6) 0.3872(6) 0.047(3) Uani 1 1 d . . .
H4 H 0.7668 -0.1700 0.3982 0.056 Uiso 1 1 calc R . .
C5 C 0.8288(13) -0.0756(6) 0.4268(6) 0.045(3) Uani 1 1 d . . .
H5 H 0.7852 -0.0720 0.4689 0.054 Uiso 1 1 calc R . .
C6 C 1.0046(11) 0.1894(5) 0.3769(5) 0.032(3) Uani 1 1 d . . .
H6 H 0.9734 0.2307 0.3446 0.038 Uiso 1 1 calc R . .
C7 C 1.1455(11) 0.1889(6) 0.3680(6) 0.039(3) Uani 1 1 d . . .
H7A H 1.1680 0.1816 0.3204 0.047 Uiso 1 1 calc R . .
H7B H 1.1805 0.1494 0.4003 0.047 Uiso 1 1 calc R . .
C8 C 1.2018(12) 0.2581(6) 0.3820(6) 0.042(3) Uani 1 1 d . . .
H8A H 1.2939 0.2558 0.3782 0.050 Uiso 1 1 calc R . .
H8B H 1.1730 0.2972 0.3471 0.050 Uiso 1 1 calc R . .
C9 C 1.1633(12) 0.2721(6) 0.4537(6) 0.040(3) Uani 1 1 d . . .
H9A H 1.2003 0.2357 0.4886 0.048 Uiso 1 1 calc R . .
H9B H 1.1963 0.3183 0.4608 0.048 Uiso 1 1 calc R . .
C10 C 1.0243(14) 0.2716(7) 0.4638(7) 0.055(4) Uani 1 1 d . . .
H10A H 0.9877 0.3112 0.4324 0.066 Uiso 1 1 calc R . .
H10B H 1.0031 0.2782 0.5118 0.066 Uiso 1 1 calc R . .
C11 C 0.9678(12) 0.2016(7) 0.4494(6) 0.045(3) Uani 1 1 d . . .
H11A H 0.9985 0.1623 0.4834 0.054 Uiso 1 1 calc R . .
H11B H 0.8758 0.2033 0.4542 0.054 Uiso 1 1 calc R . .
C12 C 0.7794(15) 0.1199(5) 0.3366(6) 0.053(4) Uani 1 1 d . . .
H12 H 0.7562 0.0763 0.3179 0.063 Uiso 1 1 calc R . .
C13 C 0.6892(11) 0.1216(7) 0.3996(6) 0.044(3) Uani 1 1 d . . .
H13A H 0.7075 0.0809 0.4353 0.052 Uiso 1 1 calc R . .
H13B H 0.7052 0.1648 0.4196 0.052 Uiso 1 1 calc R . .
C14 C 0.5540(12) 0.1196(7) 0.3820(7) 0.049(3) Uani 1 1 d . . .
H14A H 0.5019 0.1230 0.4237 0.059 Uiso 1 1 calc R . .
H14B H 0.5352 0.0743 0.3665 0.059 Uiso 1 1 calc R . .
C15 C 0.5218(13) 0.1802(7) 0.3252(7) 0.053(3) Uani 1 1 d . . .
H15A H 0.5305 0.2254 0.3427 0.064 Uiso 1 1 calc R . .
H15B H 0.4341 0.1756 0.3118 0.064 Uiso 1 1 calc R . .
C16 C 0.6081(12) 0.1797(8) 0.2620(7) 0.054(4) Uani 1 1 d . . .
H16A H 0.5916 0.1369 0.2414 0.065 Uiso 1 1 calc R . .
H16B H 0.5890 0.2210 0.2271 0.065 Uiso 1 1 calc R . .
C17 C 0.7431(13) 0.1814(7) 0.2791(7) 0.051(3) Uani 1 1 d . . .
H17A H 0.7619 0.2267 0.2946 0.061 Uiso 1 1 calc R . .
H17B H 0.7943 0.1785 0.2370 0.061 Uiso 1 1 calc R . .
C18 C 0.9452(12) -0.0268(6) 0.0908(5) 0.040(3) Uani 1 1 d . . .
H18A H 0.9099 -0.0438 0.0502 0.048 Uiso 1 1 calc R . .
H18B H 1.0011 0.0133 0.0740 0.048 Uiso 1 1 calc R . .
C19 C 1.0183(12) -0.0848(6) 0.1319(5) 0.036(3) Uani 1 1 d . . .
C20 C 1.1351(12) -0.1372(6) 0.2151(6) 0.041(3) Uani 1 1 d . . .
H20 H 1.1806 -0.1462 0.2565 0.050 Uiso 1 1 calc R . .
C21 C 1.1253(13) -0.1828(6) 0.1686(7) 0.045(3) Uani 1 1 d . . .
H21 H 1.1619 -0.2281 0.1709 0.054 Uiso 1 1 calc R . .
C22 C 1.0482(13) -0.1478(7) 0.1159(7) 0.051(4) Uani 1 1 d . . .
H22 H 1.0226 -0.1661 0.0761 0.061 Uiso 1 1 calc R . .
C23 C 0.7221(12) -0.0729(6) 0.1705(6) 0.040(3) Uani 1 1 d . . .
H23 H 0.7761 -0.1069 0.2002 0.048 Uiso 1 1 calc R . .
C24 C 0.6778(14) -0.1138(6) 0.1147(7) 0.051(3) Uani 1 1 d . . .
H24A H 0.6248 -0.0829 0.0822 0.061 Uiso 1 1 calc R . .
H24B H 0.7509 -0.1281 0.0884 0.061 Uiso 1 1 calc R . .
C25 C 0.6040(13) -0.1788(6) 0.1458(7) 0.050(3) Uani 1 1 d . . .
H25A H 0.5711 -0.2015 0.1079 0.061 Uiso 1 1 calc R . .
H25B H 0.6609 -0.2126 0.1726 0.061 Uiso 1 1 calc R . .
C26 C 0.4988(14) -0.1636(7) 0.1913(8) 0.060(4) Uani 1 1 d . . .
H26A H 0.4582 -0.2082 0.2123 0.073 Uiso 1 1 calc R . .
H26B H 0.4361 -0.1344 0.1638 0.073 Uiso 1 1 calc R . .
C27 C 0.5459(19) -0.1242(7) 0.2492(7) 0.079(6) Uani 1 1 d . . .
H27A H 0.4741 -0.1121 0.2777 0.094 Uiso 1 1 calc R . .
H27B H 0.6022 -0.1554 0.2795 0.094 Uiso 1 1 calc R . .
C28 C 0.6156(16) -0.0573(7) 0.2185(8) 0.065(4) Uani 1 1 d . . .
H28A H 0.5567 -0.0239 0.1926 0.078 Uiso 1 1 calc R . .
H28B H 0.6492 -0.0347 0.2563 0.078 Uiso 1 1 calc R . .
C29 C 0.7302(14) 0.0733(7) 0.0974(7) 0.054(4) Uani 1 1 d . . .
H29 H 0.6655 0.0848 0.1315 0.065 Uiso 1 1 calc R . .
C30 C 0.8113(19) 0.1387(7) 0.0804(11) 0.096(7) Uani 1 1 d . . .
H30A H 0.8756 0.1315 0.0451 0.115 Uiso 1 1 calc R . .
H30B H 0.8540 0.1479 0.1223 0.115 Uiso 1 1 calc R . .
C31 C 0.724(3) 0.2048(9) 0.0516(11) 0.116(8) Uani 1 1 d . . .
H31A H 0.6645 0.2142 0.0884 0.139 Uiso 1 1 calc R . .
H31B H 0.7765 0.2472 0.0384 0.139 Uiso 1 1 calc R . .
C32 C 0.6589(19) 0.1914(8) -0.0051(9) 0.084(6) Uani 1 1 d . . .
H32A H 0.7179 0.1810 -0.0417 0.101 Uiso 1 1 calc R . .
H32B H 0.6093 0.2333 -0.0237 0.101 Uiso 1 1 calc R . .
C33 C 0.574(3) 0.1297(11) 0.0166(15) 0.171(15) Uani 1 1 d . . .
H33A H 0.5205 0.1218 -0.0220 0.206 Uiso 1 1 calc R . .
H33B H 0.5195 0.1380 0.0561 0.206 Uiso 1 1 calc R . .
C34 C 0.664(3) 0.0616(9) 0.0389(13) 0.141(11) Uani 1 1 d . . .
H34A H 0.6135 0.0183 0.0499 0.169 Uiso 1 1 calc R . .
H34B H 0.7232 0.0559 0.0006 0.169 Uiso 1 1 calc R . .
C35 C 1.2482(12) 0.0436(7) 0.1303(7) 0.054(4) Uani 1 1 d . . .
H35A H 1.2239 0.0464 0.0821 0.081 Uiso 1 1 calc R . .
H35B H 1.2664 -0.0054 0.1493 0.081 Uiso 1 1 calc R . .
H35C H 1.3225 0.0724 0.1326 0.081 Uiso 1 1 calc R . .
C36 C 1.1295(14) 0.1442(6) 0.1479(7) 0.054(4) Uani 1 1 d . . .
H36A H 1.2004 0.1698 0.1625 0.081 Uiso 1 1 calc R . .
H36B H 1.0522 0.1598 0.1685 0.081 Uiso 1 1 calc R . .
H36C H 1.1247 0.1534 0.0975 0.081 Uiso 1 1 calc R . .
C37 C 1.2203(12) -0.0615(6) 0.3629(6) 0.043(3) Uani 1 1 d . . .
H37A H 1.2941 -0.0900 0.3560 0.065 Uiso 1 1 calc R . .
H37B H 1.1462 -0.0916 0.3690 0.065 Uiso 1 1 calc R . .
H37C H 1.2306 -0.0391 0.4040 0.065 Uiso 1 1 calc R . .
C38 C 1.3126(12) 0.0386(6) 0.2967(7) 0.051(3) Uani 1 1 d . . .
H38A H 1.3228 0.0565 0.3404 0.077 Uiso 1 1 calc R . .
H38B H 1.3007 0.0781 0.2596 0.077 Uiso 1 1 calc R . .
H38C H 1.3873 0.0123 0.2865 0.077 Uiso 1 1 calc R . .
Ti2 Ti 0.46519(19) 0.51043(9) 0.24198(10) 0.0286(5) Uani 1 1 d . . .
N5 N 0.4560(9) 0.4225(4) 0.1929(4) 0.031(2) Uani 1 1 d . . .
N6 N 0.5664(9) 0.4512(4) 0.3260(5) 0.035(2) Uani 1 1 d . . .
N7 N 0.3814(9) 0.5675(5) 0.1676(5) 0.038(2) Uani 1 1 d . . .
N8 N 0.3177(9) 0.4933(4) 0.3005(5) 0.037(2) Uani 1 1 d . . .
O3 O 0.6466(7) 0.5283(3) 0.1936(4) 0.0319(18) Uani 1 1 d . . .
O4 O 0.5176(7) 0.5996(3) 0.2781(3) 0.0289(17) Uani 1 1 d . . .
P3 P 0.7072(3) 0.49816(15) 0.13370(14) 0.0327(7) Uani 1 1 d . . .
P4 P 0.5761(3) 0.61024(14) 0.34607(14) 0.0296(7) Uani 1 1 d . . .
C39 C 0.5857(11) 0.4648(6) 0.0854(5) 0.036(3) Uani 1 1 d . . .
H39A H 0.5302 0.5039 0.0663 0.043 Uiso 1 1 calc R . .
H39B H 0.6233 0.4444 0.0464 0.043 Uiso 1 1 calc R . .
C40 C 0.5108(11) 0.4095(6) 0.1311(6) 0.035(3) Uani 1 1 d . . .
C41 C 0.3899(12) 0.3606(6) 0.2170(6) 0.039(3) Uani 1 1 d . . .
H41 H 0.3429 0.3529 0.2591 0.047 Uiso 1 1 calc R . .
C42 C 0.4011(12) 0.3136(6) 0.1732(7) 0.043(3) Uani 1 1 d . . .
H42 H 0.3637 0.2684 0.1786 0.052 Uiso 1 1 calc R . .
C43 C 0.4781(12) 0.3437(6) 0.1182(6) 0.043(3) Uani 1 1 d . . .
H43 H 0.5032 0.3227 0.0793 0.051 Uiso 1 1 calc R . .
C44 C 0.7898(12) 0.5653(6) 0.0742(6) 0.040(3) Uani 1 1 d . . .
H44 H 0.8257 0.5428 0.0355 0.048 Uiso 1 1 calc R . .
C45 C 0.7020(14) 0.6231(7) 0.0441(7) 0.058(4) Uani 1 1 d . . .
H45A H 0.6593 0.6426 0.0823 0.069 Uiso 1 1 calc R . .
H45B H 0.6376 0.6028 0.0177 0.069 Uiso 1 1 calc R . .
C46 C 0.7677(16) 0.6823(7) -0.0029(8) 0.065(4) Uani 1 1 d . . .
H46A H 0.8030 0.6643 -0.0439 0.078 Uiso 1 1 calc R . .
H46B H 0.7066 0.7196 -0.0191 0.078 Uiso 1 1 calc R . .
C47 C 0.8708(14) 0.7131(7) 0.0341(7) 0.055(4) Uani 1 1 d . . .
H47A H 0.8346 0.7358 0.0720 0.066 Uiso 1 1 calc R . .
H47B H 0.9158 0.7494 0.0016 0.066 Uiso 1 1 calc R . .
C48 C 0.9613(13) 0.6560(6) 0.0633(7) 0.052(3) Uani 1 1 d . . .
H48A H 1.0055 0.6377 0.0249 0.063 Uiso 1 1 calc R . .
H48B H 1.0243 0.6763 0.0907 0.063 Uiso 1 1 calc R . .
C49 C 0.8945(14) 0.5963(7) 0.1085(7) 0.055(4) Uani 1 1 d . . .
H49A H 0.9557 0.5587 0.1236 0.066 Uiso 1 1 calc R . .
H49B H 0.8612 0.6136 0.1503 0.066 Uiso 1 1 calc R . .
C50 C 0.8038(11) 0.4247(5) 0.1646(5) 0.030(3) Uani 1 1 d . . .
H50 H 0.7455 0.3867 0.1861 0.036 Uiso 1 1 calc R . .
C51 C 0.8908(13) 0.4383(6) 0.2226(6) 0.040(3) Uani 1 1 d . . .
H51A H 0.8415 0.4564 0.2594 0.048 Uiso 1 1 calc R . .
H51B H 0.9533 0.4744 0.2039 0.048 Uiso 1 1 calc R . .
C52 C 0.9581(13) 0.3698(6) 0.2531(7) 0.046(3) Uani 1 1 d . . .
H52A H 1.0179 0.3803 0.2879 0.056 Uiso 1 1 calc R . .
H52B H 0.8960 0.3359 0.2768 0.056 Uiso 1 1 calc R . .
C53 C 1.0256(12) 0.3376(7) 0.1993(7) 0.050(3) Uani 1 1 d . . .
H53A H 1.0625 0.2925 0.2207 0.060 Uiso 1 1 calc R . .
H53B H 1.0947 0.3690 0.1799 0.060 Uiso 1 1 calc R . .
C54 C 0.9433(12) 0.3243(6) 0.1415(6) 0.044(3) Uani 1 1 d . . .
H54A H 0.8787 0.2892 0.1597 0.053 Uiso 1 1 calc R . .
H54B H 0.9939 0.3048 0.1060 0.053 Uiso 1 1 calc R . .
C55 C 0.8801(13) 0.3931(6) 0.1087(6) 0.043(3) Uani 1 1 d . . .
H55A H 0.8243 0.3835 0.0717 0.051 Uiso 1 1 calc R . .
H55B H 0.9444 0.4272 0.0877 0.051 Uiso 1 1 calc R . .
C56 C 0.5432(12) 0.5353(5) 0.4110(5) 0.035(3) Uani 1 1 d . . .
H56A H 0.5811 0.5423 0.4550 0.042 Uiso 1 1 calc R . .
H56B H 0.4519 0.5305 0.4188 0.042 Uiso 1 1 calc R . .
C57 C 0.5941(11) 0.4703(5) 0.3887(5) 0.031(3) Uani 1 1 d . . .
C58 C 0.6245(12) 0.3881(5) 0.3246(6) 0.038(3) Uani 1 1 d . . .
H58 H 0.6197 0.3616 0.2877 0.046 Uiso 1 1 calc R . .
C59 C 0.6909(13) 0.3681(6) 0.3834(6) 0.046(3) Uani 1 1 d . . .
H59 H 0.7397 0.3267 0.3938 0.055 Uiso 1 1 calc R . .
C60 C 0.6728(13) 0.4206(6) 0.4252(6) 0.044(3) Uani 1 1 d . . .
H60 H 0.7071 0.4220 0.4693 0.053 Uiso 1 1 calc R . .
C61 C 0.7402(15) 0.6163(6) 0.3354(6) 0.050(4) Uani 1 1 d . . .
H61 H 0.7659 0.5733 0.3157 0.060 Uiso 1 1 calc R . .
C62 C 0.8159(14) 0.6146(9) 0.4002(7) 0.062(4) Uani 1 1 d . . .
H62A H 0.7925 0.6555 0.4228 0.075 Uiso 1 1 calc R . .
H62B H 0.7946 0.5715 0.4327 0.075 Uiso 1 1 calc R . .
C63 C 0.9545(13) 0.6161(8) 0.3859(7) 0.056(4) Uani 1 1 d . . .
H63A H 0.9985 0.6178 0.4294 0.067 Uiso 1 1 calc R . .
H63B H 0.9798 0.5723 0.3686 0.067 Uiso 1 1 calc R . .
C64 C 0.9927(13) 0.6783(7) 0.3336(8) 0.059(4) Uani 1 1 d . . .
H64A H 0.9775 0.7220 0.3531 0.070 Uiso 1 1 calc R . .
H64B H 1.0830 0.6754 0.3228 0.070 Uiso 1 1 calc R . .
C65 C 0.9212(13) 0.6806(7) 0.2686(7) 0.057(4) Uani 1 1 d . . .
H65A H 0.9428 0.7242 0.2369 0.068 Uiso 1 1 calc R . .
H65B H 0.9459 0.6402 0.2457 0.068 Uiso 1 1 calc R . .
C66 C 0.7839(12) 0.6784(6) 0.2822(7) 0.048(3) Uani 1 1 d . . .
H66A H 0.7415 0.6763 0.2382 0.057 Uiso 1 1 calc R . .
H66B H 0.7580 0.7226 0.2984 0.057 Uiso 1 1 calc R . .
C67 C 0.5060(11) 0.6894(6) 0.3715(6) 0.035(3) Uani 1 1 d . . .
H67 H 0.5401 0.7302 0.3387 0.042 Uiso 1 1 calc R . .
C68 C 0.5388(12) 0.7020(7) 0.4444(6) 0.043(3) Uani 1 1 d . . .
H68A H 0.5101 0.6615 0.4784 0.052 Uiso 1 1 calc R . .
H68B H 0.6304 0.7056 0.4476 0.052 Uiso 1 1 calc R . .
C69 C 0.4785(12) 0.7689(7) 0.4617(7) 0.050(3) Uani 1 1 d . . .
H69A H 0.4935 0.7725 0.5106 0.060 Uiso 1 1 calc R . .
H69B H 0.5181 0.8099 0.4329 0.060 Uiso 1 1 calc R . .
C70 C 0.3438(12) 0.7708(6) 0.4503(6) 0.041(3) Uani 1 1 d . . .
H70A H 0.3113 0.8175 0.4572 0.049 Uiso 1 1 calc R . .
H70B H 0.3026 0.7351 0.4852 0.049 Uiso 1 1 calc R . .
C71 C 0.3092(13) 0.7572(6) 0.3785(6) 0.042(3) Uani 1 1 d . . .
H71A H 0.2174 0.7536 0.3759 0.050 Uiso 1 1 calc R . .
H71B H 0.3376 0.7970 0.3436 0.050 Uiso 1 1 calc R . .
C72 C 0.3690(11) 0.6895(6) 0.3624(6) 0.039(3) Uani 1 1 d . . .
H72A H 0.3318 0.6490 0.3933 0.047 Uiso 1 1 calc R . .
H72B H 0.3512 0.6839 0.3143 0.047 Uiso 1 1 calc R . .
C73 C 0.4025(15) 0.6426(6) 0.1416(7) 0.053(4) Uani 1 1 d . . .
H73A H 0.4187 0.6489 0.0916 0.080 Uiso 1 1 calc R . .
H73B H 0.4745 0.6592 0.1643 0.080 Uiso 1 1 calc R . .
H73C H 0.3284 0.6696 0.1514 0.080 Uiso 1 1 calc R . .
C74 C 0.2810(12) 0.5431(7) 0.1296(7) 0.051(3) Uani 1 1 d . . .
H74A H 0.2031 0.5661 0.1408 0.077 Uiso 1 1 calc R . .
H74B H 0.2723 0.4921 0.1423 0.077 Uiso 1 1 calc R . .
H74C H 0.2995 0.5546 0.0800 0.077 Uiso 1 1 calc R . .
C75 C 0.2965(13) 0.4382(6) 0.3603(6) 0.049(3) Uani 1 1 d . . .
H75A H 0.2885 0.4598 0.4023 0.073 Uiso 1 1 calc R . .
H75B H 0.3671 0.4055 0.3643 0.073 Uiso 1 1 calc R . .
H75C H 0.2198 0.4126 0.3541 0.073 Uiso 1 1 calc R . .
C76 C 0.2052(11) 0.5373(8) 0.2936(7) 0.051(3) Uani 1 1 d . . .
H76A H 0.1335 0.5086 0.2852 0.076 Uiso 1 1 calc R . .
H76B H 0.2168 0.5755 0.2547 0.076 Uiso 1 1 calc R . .
H76C H 0.1903 0.5572 0.3361 0.076 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0375(12) 0.0197(10) 0.0292(11) -0.0041(8) 0.0000(9) -0.0020(8)
N1 0.039(6) 0.028(5) 0.028(5) -0.008(4) -0.005(4) -0.001(4)
N2 0.039(6) 0.026(5) 0.027(5) -0.010(4) 0.004(4) 0.002(4)
N3 0.053(6) 0.022(5) 0.037(6) -0.001(4) 0.007(5) -0.005(4)
N4 0.055(7) 0.031(5) 0.042(6) -0.003(4) -0.013(5) 0.003(5)
O1 0.047(5) 0.027(4) 0.022(4) -0.007(3) -0.003(3) -0.005(3)
O2 0.040(5) 0.036(4) 0.033(4) -0.006(3) -0.005(4) 0.008(4)
P1 0.0430(18) 0.0214(14) 0.0223(15) -0.0034(11) -0.0010(13) -0.0011(13)
P2 0.0451(19) 0.0289(16) 0.0327(17) 0.0003(13) -0.0043(14) -0.0045(14)
C1 0.070(9) 0.022(6) 0.029(6) 0.004(5) -0.004(6) 0.008(6)
C2 0.041(7) 0.029(6) 0.035(7) 0.001(5) -0.007(5) 0.004(5)
C3 0.084(10) 0.033(7) 0.021(6) -0.003(5) -0.006(6) -0.014(6)
C4 0.079(10) 0.026(6) 0.032(7) 0.006(5) 0.001(7) -0.013(6)
C5 0.069(9) 0.039(7) 0.025(6) 0.003(5) 0.003(6) -0.015(6)
C6 0.052(8) 0.015(5) 0.026(6) 0.000(4) -0.009(5) 0.000(5)
C7 0.042(7) 0.031(6) 0.045(7) -0.012(5) 0.005(6) -0.006(5)
C8 0.047(8) 0.032(6) 0.047(7) -0.006(5) -0.008(6) 0.000(6)
C9 0.060(9) 0.030(6) 0.030(6) -0.003(5) -0.011(6) -0.006(6)
C10 0.069(10) 0.052(8) 0.052(8) -0.031(7) -0.004(7) -0.012(7)
C11 0.037(7) 0.055(8) 0.046(7) -0.021(6) 0.002(6) -0.009(6)
C12 0.126(13) 0.013(5) 0.020(6) -0.007(4) 0.010(7) -0.021(7)
C13 0.032(7) 0.052(8) 0.048(8) -0.013(6) 0.003(6) -0.004(6)
C14 0.050(8) 0.046(8) 0.050(8) -0.010(6) 0.020(7) -0.005(6)
C15 0.042(8) 0.051(8) 0.070(9) -0.017(7) -0.005(7) 0.004(6)
C16 0.045(8) 0.059(9) 0.053(8) 0.011(7) -0.002(7) 0.004(7)
C17 0.048(8) 0.051(8) 0.049(8) 0.008(6) -0.002(6) 0.010(6)
C18 0.053(8) 0.046(7) 0.022(6) -0.009(5) 0.011(5) -0.021(6)
C19 0.058(8) 0.029(6) 0.022(6) -0.005(5) 0.005(5) -0.001(5)
C20 0.061(9) 0.024(6) 0.039(7) -0.002(5) -0.003(6) 0.003(6)
C21 0.062(9) 0.023(6) 0.052(8) -0.011(6) 0.014(7) -0.010(6)
C22 0.065(9) 0.051(8) 0.042(8) -0.029(6) 0.011(7) -0.012(7)
C23 0.055(8) 0.033(6) 0.029(6) 0.002(5) -0.002(6) -0.003(6)
C24 0.080(10) 0.030(6) 0.044(8) -0.011(5) -0.001(7) -0.011(6)
C25 0.069(10) 0.034(7) 0.048(8) -0.003(6) -0.008(7) -0.013(6)
C26 0.058(9) 0.037(7) 0.084(11) -0.005(7) 0.013(8) -0.015(7)
C27 0.137(16) 0.048(9) 0.050(9) -0.008(7) 0.041(10) -0.036(9)
C28 0.090(12) 0.038(8) 0.067(10) -0.014(7) 0.024(9) -0.022(7)
C29 0.070(10) 0.041(7) 0.047(8) 0.011(6) -0.008(7) -0.008(7)
C30 0.127(17) 0.033(8) 0.120(15) 0.024(9) -0.061(13) 0.001(9)
C31 0.20(3) 0.042(9) 0.102(15) 0.004(9) -0.045(17) -0.007(12)
C32 0.122(16) 0.055(10) 0.067(11) 0.027(8) -0.028(11) -0.013(10)
C33 0.20(3) 0.080(14) 0.21(3) 0.075(17) -0.15(2) -0.045(16)
C34 0.23(3) 0.044(10) 0.14(2) 0.018(11) -0.12(2) -0.018(13)
C35 0.046(8) 0.057(8) 0.065(9) -0.031(7) 0.015(7) -0.010(7)
C36 0.073(10) 0.035(7) 0.050(8) 0.004(6) 0.007(7) -0.002(7)
C37 0.049(8) 0.036(7) 0.046(7) -0.012(6) -0.010(6) 0.010(6)
C38 0.050(8) 0.034(7) 0.071(9) -0.009(6) -0.018(7) -0.002(6)
Ti2 0.0372(12) 0.0192(10) 0.0294(11) -0.0035(8) 0.0002(9) 0.0008(8)
N5 0.042(6) 0.020(5) 0.031(5) -0.004(4) 0.003(4) -0.005(4)
N6 0.048(6) 0.017(5) 0.038(6) -0.001(4) 0.004(5) -0.001(4)
N7 0.047(6) 0.025(5) 0.045(6) -0.012(4) -0.005(5) 0.001(4)
N8 0.048(6) 0.021(5) 0.043(6) -0.008(4) 0.008(5) -0.007(4)
O3 0.044(5) 0.022(4) 0.029(4) -0.003(3) 0.001(3) 0.001(3)
O4 0.042(5) 0.019(4) 0.025(4) -0.002(3) 0.000(3) 0.005(3)
P3 0.0441(19) 0.0294(15) 0.0241(15) -0.0024(12) -0.0006(13) 0.0019(13)
P4 0.0461(18) 0.0186(14) 0.0233(15) -0.0013(11) 0.0012(13) -0.0001(13)
C39 0.046(7) 0.041(7) 0.023(6) -0.010(5) -0.008(5) 0.000(6)
C40 0.041(7) 0.034(6) 0.030(6) -0.009(5) -0.010(5) 0.004(5)
C41 0.051(8) 0.035(7) 0.032(7) -0.006(5) -0.004(6) -0.003(6)
C42 0.046(8) 0.018(6) 0.069(9) -0.015(6) -0.014(7) -0.001(5)
C43 0.058(9) 0.027(6) 0.045(7) -0.012(5) -0.013(7) 0.003(6)
C44 0.053(8) 0.033(6) 0.031(6) 0.001(5) 0.007(6) 0.001(6)
C45 0.062(9) 0.051(8) 0.053(8) 0.018(7) -0.017(7) 0.003(7)
C46 0.092(12) 0.037(7) 0.061(9) 0.012(6) -0.021(8) -0.010(7)
C47 0.080(11) 0.038(7) 0.043(8) 0.005(6) 0.000(7) -0.013(7)
C48 0.058(9) 0.038(7) 0.055(8) 0.015(6) -0.005(7) -0.013(6)
C49 0.075(10) 0.039(7) 0.048(8) 0.011(6) -0.012(7) -0.006(7)
C50 0.040(7) 0.021(5) 0.029(6) 0.001(4) 0.000(5) 0.004(5)
C51 0.065(9) 0.022(6) 0.033(7) -0.002(5) -0.019(6) 0.001(5)
C52 0.048(8) 0.039(7) 0.051(8) -0.003(6) -0.006(6) 0.012(6)
C53 0.042(8) 0.043(7) 0.057(8) 0.018(6) 0.005(7) 0.010(6)
C54 0.042(8) 0.039(7) 0.050(8) -0.007(6) 0.015(6) 0.010(6)
C55 0.060(9) 0.032(6) 0.038(7) -0.010(5) 0.003(6) 0.011(6)
C56 0.056(8) 0.020(6) 0.029(6) -0.004(5) 0.007(5) -0.014(5)
C57 0.044(7) 0.023(6) 0.023(6) 0.006(5) 0.000(5) -0.001(5)
C58 0.071(9) 0.015(6) 0.025(6) 0.006(5) 0.016(6) 0.000(5)
C59 0.066(9) 0.035(7) 0.031(7) 0.009(5) 0.013(6) 0.017(6)
C60 0.084(10) 0.025(6) 0.021(6) 0.007(5) -0.008(6) -0.001(6)
C61 0.109(12) 0.022(6) 0.025(6) -0.014(5) -0.018(7) -0.004(7)
C62 0.070(10) 0.082(11) 0.036(8) -0.011(7) 0.000(7) 0.013(8)
C63 0.049(9) 0.077(10) 0.050(8) -0.031(7) -0.010(7) 0.007(7)
C64 0.048(8) 0.057(9) 0.080(11) -0.038(8) 0.001(8) -0.009(7)
C65 0.063(10) 0.051(8) 0.055(9) 0.001(7) 0.001(7) -0.029(7)
C66 0.053(9) 0.037(7) 0.051(8) 0.003(6) -0.009(6) -0.005(6)
C67 0.046(8) 0.033(6) 0.028(6) -0.011(5) 0.003(5) -0.006(5)
C68 0.033(7) 0.055(8) 0.045(7) -0.022(6) 0.000(6) 0.005(6)
C69 0.049(8) 0.063(9) 0.046(8) -0.036(7) 0.008(6) 0.003(7)
C70 0.064(9) 0.026(6) 0.032(7) -0.007(5) 0.008(6) 0.006(6)
C71 0.057(8) 0.027(6) 0.042(7) -0.011(5) 0.003(6) 0.002(6)
C72 0.048(8) 0.033(6) 0.037(7) -0.008(5) 0.002(6) -0.008(5)
C73 0.082(10) 0.034(7) 0.041(7) 0.006(6) -0.001(7) 0.009(7)
C74 0.049(8) 0.044(7) 0.054(8) 0.015(6) -0.007(7) 0.006(6)
C75 0.063(9) 0.035(7) 0.047(8) -0.010(6) 0.020(7) -0.003(6)
C76 0.024(7) 0.072(9) 0.058(9) -0.021(7) 0.010(6) -0.001(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N4 1.939(10) . ?
Ti1 N3 1.940(9) . ?
Ti1 O1 2.039(7) . ?
Ti1 N2 2.088(8) . ?
Ti1 O2 2.157(8) . ?
Ti1 N1 2.183(9) . ?
N1 C2 1.378(14) . ?
N1 C3 1.388(15) . ?
N2 C19 1.363(14) . ?
N2 C20 1.412(15) . ?
N3 C36 1.450(15) . ?
N3 C35 1.464(15) . ?
N4 C38 1.442(16) . ?
N4 C37 1.472(15) . ?
O1 P1 1.528(8) . ?
O2 P2 1.477(8) . ?
P1 C12 1.742(17) . ?
P1 C6 1.805(10) . ?
P1 C1 1.806(10) . ?
P2 C18 1.791(12) . ?
P2 C23 1.799(12) . ?
P2 C29 1.821(13) . ?
C1 C2 1.483(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.393(17) . ?
C3 C4 1.360(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(17) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.517(17) . ?
C6 C11 1.518(16) . ?
C6 H6 1.0000 . ?
C7 C8 1.531(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.518(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.500(19) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.547(16) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.557(17) . ?
C12 C17 1.560(17) . ?
C12 H12 1.0000 . ?
C13 C14 1.500(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.528(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.530(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.496(19) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.503(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C22 1.335(16) . ?
C20 C21 1.366(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.424(19) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.523(19) . ?
C23 C24 1.527(16) . ?
C23 H23 1.0000 . ?
C24 C25 1.523(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.479(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.55(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.526(18) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C34 1.41(2) . ?
C29 C30 1.52(2) . ?
C29 H29 1.0000 . ?
C30 C31 1.62(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.38(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.50(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.64(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
Ti2 N7 1.925(10) . ?
Ti2 N8 1.931(10) . ?
Ti2 O4 2.040(7) . ?
Ti2 N5 2.075(8) . ?
Ti2 O3 2.151(8) . ?
Ti2 N6 2.166(10) . ?
N5 C40 1.391(14) . ?
N5 C41 1.402(15) . ?
N6 C58 1.366(14) . ?
N6 C57 1.376(14) . ?
N7 C74 1.444(16) . ?
N7 C73 1.473(15) . ?
N8 C76 1.469(16) . ?
N8 C75 1.470(15) . ?
O3 P3 1.520(8) . ?
O4 P4 1.529(8) . ?
P3 C50 1.787(11) . ?
P3 C39 1.805(11) . ?
P3 C44 1.821(11) . ?
P4 C61 1.770(16) . ?
P4 C56 1.801(10) . ?
P4 C67 1.829(11) . ?
C39 C40 1.503(16) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C43 1.379(16) . ?
C41 C42 1.343(16) . ?
C41 H41 0.9500 . ?
C42 C43 1.397(18) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C49 1.494(18) . ?
C44 C45 1.513(17) . ?
C44 H44 1.0000 . ?
C45 C46 1.516(19) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.51(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.518(19) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.512(17) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.541(16) . ?
C50 C55 1.551(15) . ?
C50 H50 1.0000 . ?
C51 C52 1.546(16) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.478(17) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.505(19) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.544(16) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.485(15) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C60 1.398(16) . ?
C58 C59 1.373(18) . ?
C58 H58 0.9500 . ?
C59 C60 1.407(17) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.519(18) . ?
C61 C66 1.530(17) . ?
C61 H61 1.0000 . ?
C62 C63 1.51(2) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.50(2) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.50(2) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.490(19) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C72 1.483(17) . ?
C67 C68 1.536(16) . ?
C67 H67 1.0000 . ?
C68 C69 1.519(16) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.466(18) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.527(16) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.522(16) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ti1 N3 94.9(4) . . ?
N4 Ti1 O1 95.9(4) . . ?
N3 Ti1 O1 88.8(3) . . ?
N4 Ti1 N2 99.7(4) . . ?
N3 Ti1 N2 90.8(4) . . ?
O1 Ti1 N2 164.4(3) . . ?
N4 Ti1 O2 168.7(4) . . ?
N3 Ti1 O2 95.3(4) . . ?
O1 Ti1 O2 79.4(3) . . ?
N2 Ti1 O2 85.0(3) . . ?
N4 Ti1 N1 87.5(4) . . ?
N3 Ti1 N1 176.0(4) . . ?
O1 Ti1 N1 87.7(3) . . ?
N2 Ti1 N1 92.0(3) . . ?
O2 Ti1 N1 82.1(3) . . ?
C2 N1 C3 105.3(9) . . ?
C2 N1 Ti1 128.5(7) . . ?
C3 N1 Ti1 125.7(7) . . ?
C19 N2 C20 104.8(9) . . ?
C19 N2 Ti1 130.8(7) . . ?
C20 N2 Ti1 124.4(7) . . ?
C36 N3 C35 109.4(10) . . ?
C36 N3 Ti1 127.2(8) . . ?
C35 N3 Ti1 123.3(8) . . ?
C38 N4 C37 108.1(10) . . ?
C38 N4 Ti1 124.0(8) . . ?
C37 N4 Ti1 127.3(8) . . ?
P1 O1 Ti1 132.1(4) . . ?
P2 O2 Ti1 130.2(5) . . ?
O1 P1 C12 109.5(5) . . ?
O1 P1 C6 107.7(5) . . ?
C12 P1 C6 112.4(5) . . ?
O1 P1 C1 109.6(5) . . ?
C12 P1 C1 107.9(6) . . ?
C6 P1 C1 109.6(5) . . ?
O2 P2 C18 108.8(5) . . ?
O2 P2 C23 111.1(5) . . ?
C18 P2 C23 107.4(5) . . ?
O2 P2 C29 107.1(5) . . ?
C18 P2 C29 113.0(6) . . ?
C23 P2 C29 109.5(6) . . ?
C2 C1 P1 110.6(8) . . ?
C2 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C5 109.3(10) . . ?
N1 C2 C1 122.7(10) . . ?
C5 C2 C1 127.9(11) . . ?
C4 C3 N1 111.0(10) . . ?
C4 C3 H3 124.5 . . ?
N1 C3 H3 124.5 . . ?
C3 C4 C5 106.8(11) . . ?
C3 C4 H4 126.6 . . ?
C5 C4 H4 126.6 . . ?
C4 C5 C2 107.4(11) . . ?
C4 C5 H5 126.3 . . ?
C2 C5 H5 126.3 . . ?
C7 C6 C11 110.4(10) . . ?
C7 C6 P1 110.0(8) . . ?
C11 C6 P1 115.4(8) . . ?
C7 C6 H6 106.8 . . ?
C11 C6 H6 106.8 . . ?
P1 C6 H6 106.8 . . ?
C6 C7 C8 110.9(9) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 C7 110.3(10) . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.9(10) . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 C11 111.0(11) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C6 C11 C10 109.9(10) . . ?
C6 C11 H11A 109.7 . . ?
C10 C11 H11A 109.7 . . ?
C6 C11 H11B 109.7 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C17 108.0(11) . . ?
C13 C12 P1 119.0(9) . . ?
C17 C12 P1 114.2(9) . . ?
C13 C12 H12 104.7 . . ?
C17 C12 H12 104.7 . . ?
P1 C12 H12 104.7 . . ?
C14 C13 C12 113.5(11) . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 C15 111.0(11) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 110.6(11) . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 112.7(12) . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 C12 112.2(12) . . ?
C16 C17 H17A 109.2 . . ?
C12 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
C12 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 P2 110.2(7) . . ?
C19 C18 H18A 109.6 . . ?
P2 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
P2 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C22 C19 N2 111.5(11) . . ?
C22 C19 C18 128.6(11) . . ?
N2 C19 C18 119.9(9) . . ?
C21 C20 N2 110.4(11) . . ?
C21 C20 H20 124.8 . . ?
N2 C20 H20 124.8 . . ?
C20 C21 C22 105.1(11) . . ?
C20 C21 H21 127.5 . . ?
C22 C21 H21 127.5 . . ?
C19 C22 C21 108.2(11) . . ?
C19 C22 H22 125.9 . . ?
C21 C22 H22 125.9 . . ?
C28 C23 C24 111.9(11) . . ?
C28 C23 P2 113.2(8) . . ?
C24 C23 P2 117.1(8) . . ?
C28 C23 H23 104.4 . . ?
C24 C23 H23 104.4 . . ?
P2 C23 H23 104.4 . . ?
C25 C24 C23 111.5(10) . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C26 C25 C24 113.5(11) . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 110.3(12) . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C26 110.9(12) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C23 C28 C27 111.3(11) . . ?
C23 C28 H28A 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C23 C28 H28B 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C34 C29 C30 110.4(14) . . ?
C34 C29 P2 118.8(12) . . ?
C30 C29 P2 109.5(10) . . ?
C34 C29 H29 105.7 . . ?
C30 C29 H29 105.7 . . ?
P2 C29 H29 105.7 . . ?
C29 C30 C31 108.9(16) . . ?
C29 C30 H30A 109.9 . . ?
C31 C30 H30A 109.9 . . ?
C29 C30 H30B 109.9 . . ?
C31 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
C32 C31 C30 110.7(16) . . ?
C32 C31 H31A 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
C31 C32 C33 109.0(17) . . ?
C31 C32 H32A 109.9 . . ?
C33 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C33 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C32 C33 C34 106(2) . . ?
C32 C33 H33A 110.4 . . ?
C34 C33 H33A 110.4 . . ?
C32 C33 H33B 110.4 . . ?
C34 C33 H33B 110.4 . . ?
H33A C33 H33B 108.6 . . ?
C29 C34 C33 107.9(18) . . ?
C29 C34 H34A 110.1 . . ?
C33 C34 H34A 110.1 . . ?
C29 C34 H34B 110.1 . . ?
C33 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C36 H36A 109.5 . . ?
N3 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N3 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C37 H37A 109.5 . . ?
N4 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N4 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N4 C38 H38A 109.5 . . ?
N4 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N4 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N7 Ti2 N8 95.0(4) . . ?
N7 Ti2 O4 89.3(3) . . ?
N8 Ti2 O4 95.8(3) . . ?
N7 Ti2 N5 91.7(4) . . ?
N8 Ti2 N5 98.6(4) . . ?
O4 Ti2 N5 165.4(3) . . ?
N7 Ti2 O3 93.6(4) . . ?
N8 Ti2 O3 169.9(4) . . ?
O4 Ti2 O3 79.1(3) . . ?
N5 Ti2 O3 86.4(3) . . ?
N7 Ti2 N6 176.8(4) . . ?
N8 Ti2 N6 86.7(4) . . ?
O4 Ti2 N6 87.8(3) . . ?
N5 Ti2 N6 90.7(3) . . ?
O3 Ti2 N6 84.4(3) . . ?
C40 N5 C41 103.8(8) . . ?
C40 N5 Ti2 130.4(7) . . ?
C41 N5 Ti2 125.8(7) . . ?
C58 N6 C57 105.7(9) . . ?
C58 N6 Ti2 125.8(8) . . ?
C57 N6 Ti2 128.3(7) . . ?
C74 N7 C73 108.3(10) . . ?
C74 N7 Ti2 124.3(7) . . ?
C73 N7 Ti2 127.3(8) . . ?
C76 N8 C75 107.2(10) . . ?
C76 N8 Ti2 124.3(8) . . ?
C75 N8 Ti2 128.5(8) . . ?
P3 O3 Ti2 130.7(4) . . ?
P4 O4 Ti2 131.2(4) . . ?
O3 P3 C50 110.6(5) . . ?
O3 P3 C39 108.3(5) . . ?
C50 P3 C39 106.4(5) . . ?
O3 P3 C44 111.7(5) . . ?
C50 P3 C44 112.8(6) . . ?
C39 P3 C44 106.7(5) . . ?
O4 P4 C61 109.9(5) . . ?
O4 P4 C56 109.7(5) . . ?
C61 P4 C56 107.2(6) . . ?
O4 P4 C67 107.0(5) . . ?
C61 P4 C67 112.9(5) . . ?
C56 P4 C67 110.2(5) . . ?
C40 C39 P3 110.4(8) . . ?
C40 C39 H39A 109.6 . . ?
P3 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
P3 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
C43 C40 N5 110.3(10) . . ?
C43 C40 C39 128.0(11) . . ?
N5 C40 C39 121.5(9) . . ?
C42 C41 N5 111.6(11) . . ?
C42 C41 H41 124.2 . . ?
N5 C41 H41 124.2 . . ?
C41 C42 C43 107.2(10) . . ?
C41 C42 H42 126.4 . . ?
C43 C42 H42 126.4 . . ?
C40 C43 C42 107.0(11) . . ?
C40 C43 H43 126.5 . . ?
C42 C43 H43 126.5 . . ?
C49 C44 C45 109.6(11) . . ?
C49 C44 P3 111.5(8) . . ?
C45 C44 P3 111.1(9) . . ?
C49 C44 H44 108.2 . . ?
C45 C44 H44 108.2 . . ?
P3 C44 H44 108.2 . . ?
C44 C45 C46 113.1(12) . . ?
C44 C45 H45A 109.0 . . ?
C46 C45 H45A 109.0 . . ?
C44 C45 H45B 109.0 . . ?
C46 C45 H45B 109.0 . . ?
H45A C45 H45B 107.8 . . ?
C47 C46 C45 111.0(11) . . ?
C47 C46 H46A 109.4 . . ?
C45 C46 H46A 109.4 . . ?
C47 C46 H46B 109.4 . . ?
C45 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C46 C47 C48 110.4(11) . . ?
C46 C47 H47A 109.6 . . ?
C48 C47 H47A 109.6 . . ?
C46 C47 H47B 109.6 . . ?
C48 C47 H47B 109.6 . . ?
H47A C47 H47B 108.1 . . ?
C49 C48 C47 111.3(12) . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48B 109.4 . . ?
C47 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C44 C49 C48 114.1(11) . . ?
C44 C49 H49A 108.7 . . ?
C48 C49 H49A 108.7 . . ?
C44 C49 H49B 108.7 . . ?
C48 C49 H49B 108.7 . . ?
H49A C49 H49B 107.6 . . ?
C51 C50 C55 109.5(10) . . ?
C51 C50 P3 113.6(7) . . ?
C55 C50 P3 115.7(7) . . ?
C51 C50 H50 105.8 . . ?
C55 C50 H50 105.8 . . ?
P3 C50 H50 105.8 . . ?
C50 C51 C52 110.4(9) . . ?
C50 C51 H51A 109.6 . . ?
C52 C51 H51A 109.6 . . ?
C50 C51 H51B 109.6 . . ?
C52 C51 H51B 109.6 . . ?
H51A C51 H51B 108.1 . . ?
C53 C52 C51 111.9(10) . . ?
C53 C52 H52A 109.2 . . ?
C51 C52 H52A 109.2 . . ?
C53 C52 H52B 109.2 . . ?
C51 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
C52 C53 C54 113.0(11) . . ?
C52 C53 H53A 109.0 . . ?
C54 C53 H53A 109.0 . . ?
C52 C53 H53B 109.0 . . ?
C54 C53 H53B 109.0 . . ?
H53A C53 H53B 107.8 . . ?
C53 C54 C55 110.4(10) . . ?
C53 C54 H54A 109.6 . . ?
C55 C54 H54A 109.6 . . ?
C53 C54 H54B 109.6 . . ?
C55 C54 H54B 109.6 . . ?
H54A C54 H54B 108.1 . . ?
C54 C55 C50 109.6(9) . . ?
C54 C55 H55A 109.7 . . ?
C50 C55 H55A 109.7 . . ?
C54 C55 H55B 109.7 . . ?
C50 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C57 C56 P4 110.2(7) . . ?
C57 C56 H56A 109.6 . . ?
P4 C56 H56A 109.6 . . ?
C57 C56 H56B 109.6 . . ?
P4 C56 H56B 109.6 . . ?
H56A C56 H56B 108.1 . . ?
N6 C57 C60 110.3(9) . . ?
N6 C57 C56 122.1(10) . . ?
C60 C57 C56 127.6(10) . . ?
N6 C58 C59 111.2(10) . . ?
N6 C58 H58 124.4 . . ?
C59 C58 H58 124.4 . . ?
C58 C59 C60 106.9(10) . . ?
C58 C59 H59 126.5 . . ?
C60 C59 H59 126.5 . . ?
C57 C60 C59 105.8(10) . . ?
C57 C60 H60 127.1 . . ?
C59 C60 H60 127.1 . . ?
C62 C61 C66 108.8(11) . . ?
C62 C61 P4 117.3(10) . . ?
C66 C61 P4 113.7(9) . . ?
C62 C61 H61 105.3 . . ?
C66 C61 H61 105.3 . . ?
P4 C61 H61 105.3 . . ?
C63 C62 C61 113.0(12) . . ?
C63 C62 H62A 109.0 . . ?
C61 C62 H62A 109.0 . . ?
C63 C62 H62B 109.0 . . ?
C61 C62 H62B 109.0 . . ?
H62A C62 H62B 107.8 . . ?
C64 C63 C62 111.9(13) . . ?
C64 C63 H63A 109.2 . . ?
C62 C63 H63A 109.2 . . ?
C64 C63 H63B 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C65 C64 C63 111.1(11) . . ?
C65 C64 H64A 109.4 . . ?
C63 C64 H64A 109.4 . . ?
C65 C64 H64B 109.4 . . ?
C63 C64 H64B 109.4 . . ?
H64A C64 H64B 108.0 . . ?
C66 C65 C64 112.1(12) . . ?
C66 C65 H65A 109.2 . . ?
C64 C65 H65A 109.2 . . ?
C66 C65 H65B 109.2 . . ?
C64 C65 H65B 109.2 . . ?
H65A C65 H65B 107.9 . . ?
C65 C66 C61 114.1(11) . . ?
C65 C66 H66A 108.7 . . ?
C61 C66 H66A 108.7 . . ?
C65 C66 H66B 108.7 . . ?
C61 C66 H66B 108.7 . . ?
H66A C66 H66B 107.6 . . ?
C72 C67 C68 111.3(10) . . ?
C72 C67 P4 110.7(8) . . ?
C68 C67 P4 114.2(8) . . ?
C72 C67 H67 106.7 . . ?
C68 C67 H67 106.7 . . ?
P4 C67 H67 106.7 . . ?
C69 C68 C67 111.3(11) . . ?
C69 C68 H68A 109.4 . . ?
C67 C68 H68A 109.4 . . ?
C69 C68 H68B 109.4 . . ?
C67 C68 H68B 109.4 . . ?
H68A C68 H68B 108.0 . . ?
C70 C69 C68 112.4(10) . . ?
C70 C69 H69A 109.1 . . ?
C68 C69 H69A 109.1 . . ?
C70 C69 H69B 109.1 . . ?
C68 C69 H69B 109.1 . . ?
H69A C69 H69B 107.8 . . ?
C69 C70 C71 113.5(10) . . ?
C69 C70 H70A 108.9 . . ?
C71 C70 H70A 108.9 . . ?
C69 C70 H70B 108.9 . . ?
C71 C70 H70B 108.9 . . ?
H70A C70 H70B 107.7 . . ?
C72 C71 C70 110.8(10) . . ?
C72 C71 H71A 109.5 . . ?
C70 C71 H71A 109.5 . . ?
C72 C71 H71B 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 108.1 . . ?
C67 C72 C71 111.8(10) . . ?
C67 C72 H72A 109.3 . . ?
C71 C72 H72A 109.3 . . ?
C67 C72 H72B 109.3 . . ?
C71 C72 H72B 109.3 . . ?
H72A C72 H72B 107.9 . . ?
N7 C73 H73A 109.5 . . ?
N7 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
N7 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N7 C74 H74A 109.5 . . ?
N7 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
N7 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N8 C75 H75A 109.5 . . ?
N8 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N8 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N8 C76 H76A 109.5 . . ?
N8 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
N8 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 22.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 2.670
_refine_diff_density_min -0.604
_refine_diff_density_rms 0.126
#==END
data_7b
_database_code_depnum_ccdc_archive 'CCDC 729821'
_chemical_name_common 'Compound 7b'
_chemical_melting_point ?
_chemical_formula_structural '[2-(t-Bu)-Pyr-P(O)Ph2]2Zn.PhMe'
_chemical_formula_moiety 'C42 H46 N2 O2 P2 Zn, C7 H8'
_chemical_formula_sum 'C49 H54 N2 O2 P2 Zn'
_chemical_formula_weight 830.25
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.2743(8)
_cell_length_b 11.3563(8)
_cell_length_c 18.7268(13)
_cell_angle_alpha 81.072(6)
_cell_angle_beta 75.302(6)
_cell_angle_gamma 74.362(6)
_cell_volume 2223.6(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 140(2)
_cell_measurement_reflns_used 5857
_cell_measurement_theta_min 3.5659
_cell_measurement_theta_max 27.4998
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.240
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 876
_exptl_absorpt_coefficient_mu 0.664
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8074
_exptl_absorpt_correction_T_max 0.9613
_exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 140(2)
_diffrn_radiation_probe x-ray
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method 'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 30544
_diffrn_reflns_av_R_equivalents 0.0927
_diffrn_reflns_av_sigmaI/netI 0.1768
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 3.59
_diffrn_reflns_theta_max 27.70
_reflns_number_total 10334
_reflns_number_gt 4876
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution 'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
Crystals of 5d were weakly diffracting and exhibited twinning. The
SHELX TWIN instruction used had a twin matrix [ 1 0 0 0 -1 0 0 0 -1 ]
with BASF parameters 0.09987, 0.20000 and 0.09667.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10334
_refine_ls_number_parameters 500
_refine_ls_number_restraints 57
_refine_ls_R_factor_all 0.1260
_refine_ls_R_factor_gt 0.0595
_refine_ls_wR_factor_ref 0.1648
_refine_ls_wR_factor_gt 0.1432
_refine_ls_goodness_of_fit_ref 0.874
_refine_ls_restrained_S_all 0.874
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.71460(4) 0.11104(4) 0.20974(3) 0.02444(15) Uani 1 1 d . . .
N1 N 0.6323(3) -0.0254(3) 0.23842(18) 0.0259(8) Uani 1 1 d . . .
N2 N 0.8842(3) 0.1289(3) 0.17131(18) 0.0239(8) Uani 1 1 d . . .
O1 O 0.6089(2) 0.2238(2) 0.28775(15) 0.0259(6) Uani 1 1 d . . .
O2 O 0.6378(2) 0.2191(3) 0.12567(15) 0.0279(7) Uani 1 1 d . . .
P1 P 0.46952(10) 0.23393(10) 0.30941(6) 0.0253(3) Uani 1 1 d . . .
P2 P 0.71374(10) 0.21919(10) 0.04729(6) 0.0250(3) Uani 1 1 d . . .
C1 C 0.4271(4) 0.1369(4) 0.2576(2) 0.0293(10) Uani 1 1 d . . .
H1A H 0.3361 0.1392 0.2758 0.035 Uiso 1 1 calc R . .
H1B H 0.4407 0.1696 0.2048 0.035 Uiso 1 1 calc R . .
C2 C 0.5021(4) 0.0059(4) 0.2636(2) 0.0233(9) Uani 1 1 d . . .
C3 C 0.6691(4) -0.1527(4) 0.2491(2) 0.0291(10) Uani 1 1 d . . .
C4 C 0.5633(5) -0.1976(4) 0.2809(2) 0.0375(11) Uani 1 1 d . . .
H4 H 0.5620 -0.2815 0.2942 0.045 Uiso 1 1 calc R . .
C5 C 0.4588(4) -0.0974(4) 0.2899(2) 0.0346(11) Uani 1 1 d . . .
H5 H 0.3734 -0.1005 0.3106 0.042 Uiso 1 1 calc R . .
C6 C 0.8027(5) -0.2262(4) 0.2270(3) 0.0373(11) Uani 1 1 d . . .
C7 C 0.8553(5) -0.2003(5) 0.1423(3) 0.0557(14) Uani 1 1 d . . .
H7A H 0.7993 -0.2167 0.1147 0.084 Uiso 1 1 calc R . .
H7B H 0.9400 -0.2537 0.1278 0.084 Uiso 1 1 calc R . .
H7C H 0.8598 -0.1142 0.1311 0.084 Uiso 1 1 calc R . .
C8 C 0.8909(5) -0.1968(5) 0.2676(4) 0.0659(17) Uani 1 1 d . . .
H8A H 0.8926 -0.1101 0.2557 0.099 Uiso 1 1 calc R . .
H8B H 0.9762 -0.2483 0.2520 0.099 Uiso 1 1 calc R . .
H8C H 0.8605 -0.2132 0.3211 0.099 Uiso 1 1 calc R . .
C9 C 0.8101(6) -0.3650(4) 0.2420(3) 0.0663(18) Uani 1 1 d . . .
H9A H 0.7843 -0.3864 0.2955 0.099 Uiso 1 1 calc R . .
H9B H 0.8970 -0.4110 0.2236 0.099 Uiso 1 1 calc R . .
H9C H 0.7536 -0.3860 0.2166 0.099 Uiso 1 1 calc R . .
C10 C 0.3863(4) 0.3907(4) 0.2903(2) 0.0278(10) Uani 1 1 d . . .
C11 C 0.4516(5) 0.4679(4) 0.2413(3) 0.0433(12) Uani 1 1 d . . .
H11 H 0.5382 0.4377 0.2190 0.052 Uiso 1 1 calc R . .
C12 C 0.3919(5) 0.5892(5) 0.2244(3) 0.0501(14) Uani 1 1 d . . .
H12 H 0.4373 0.6421 0.1908 0.060 Uiso 1 1 calc R . .
C13 C 0.2665(5) 0.6323(5) 0.2565(3) 0.0542(14) Uani 1 1 d . . .
H13 H 0.2251 0.7152 0.2449 0.065 Uiso 1 1 calc R . .
C14 C 0.2003(5) 0.5564(5) 0.3054(3) 0.0593(16) Uani 1 1 d . . .
H14 H 0.1138 0.5870 0.3278 0.071 Uiso 1 1 calc R . .
C15 C 0.2598(5) 0.4358(5) 0.3217(3) 0.0480(13) Uani 1 1 d . . .
H15 H 0.2137 0.3832 0.3549 0.058 Uiso 1 1 calc R . .
C16 C 0.4226(4) 0.1887(4) 0.4069(2) 0.0272(9) Uani 1 1 d . . .
C17 C 0.5014(5) 0.1958(4) 0.4515(3) 0.0380(11) Uani 1 1 d . . .
H17 H 0.5748 0.2260 0.4308 0.046 Uiso 1 1 calc R . .
C18 C 0.4718(5) 0.1581(5) 0.5270(3) 0.0456(13) Uani 1 1 d . . .
H18 H 0.5256 0.1623 0.5577 0.055 Uiso 1 1 calc R . .
C19 C 0.3657(5) 0.1149(4) 0.5572(3) 0.0455(13) Uani 1 1 d . . .
H19 H 0.3465 0.0890 0.6087 0.055 Uiso 1 1 calc R . .
C20 C 0.2874(5) 0.1091(5) 0.5135(3) 0.0469(13) Uani 1 1 d . . .
H20 H 0.2135 0.0800 0.5349 0.056 Uiso 1 1 calc R . .
C21 C 0.3148(4) 0.1455(4) 0.4378(2) 0.0368(11) Uani 1 1 d . . .
H21 H 0.2603 0.1408 0.4076 0.044 Uiso 1 1 calc R . .
C22 C 0.8623(4) 0.1073(4) 0.0428(2) 0.0246(9) Uani 1 1 d . . .
H22A H 0.8459 0.0243 0.0549 0.030 Uiso 1 1 calc R . .
H22B H 0.9133 0.1115 -0.0087 0.030 Uiso 1 1 calc R . .
C23 C 0.9373(4) 0.1246(4) 0.0942(2) 0.0240(9) Uani 1 1 d . . .
C24 C 0.9763(4) 0.1480(4) 0.2011(2) 0.0264(9) Uani 1 1 d . . .
C25 C 1.0832(4) 0.1532(4) 0.1457(2) 0.0289(10) Uani 1 1 d . . .
H25 H 1.1603 0.1645 0.1520 0.035 Uiso 1 1 calc R . .
C26 C 1.0571(4) 0.1387(4) 0.0785(2) 0.0282(10) Uani 1 1 d . . .
H26 H 1.1129 0.1388 0.0310 0.034 Uiso 1 1 calc R . .
C27 C 0.9515(4) 0.1777(4) 0.2813(2) 0.0280(10) Uani 1 1 d . . .
C28 C 0.8681(4) 0.3090(4) 0.2882(3) 0.0394(12) Uani 1 1 d . . .
H28A H 0.9113 0.3668 0.2542 0.059 Uiso 1 1 calc R . .
H28B H 0.8526 0.3297 0.3392 0.059 Uiso 1 1 calc R . .
H28C H 0.7875 0.3140 0.2758 0.059 Uiso 1 1 calc R . .
C29 C 0.8861(4) 0.0892(4) 0.3369(2) 0.0355(11) Uani 1 1 d . . .
H29A H 0.8047 0.0927 0.3259 0.053 Uiso 1 1 calc R . .
H29B H 0.8721 0.1125 0.3872 0.053 Uiso 1 1 calc R . .
H29C H 0.9394 0.0055 0.3334 0.053 Uiso 1 1 calc R . .
C30 C 1.0745(4) 0.1739(5) 0.3015(3) 0.0452(13) Uani 1 1 d . . .
H30A H 1.1308 0.0918 0.2958 0.068 Uiso 1 1 calc R . .
H30B H 1.0572 0.1924 0.3531 0.068 Uiso 1 1 calc R . .
H30C H 1.1149 0.2348 0.2687 0.068 Uiso 1 1 calc R . .
C31 C 0.6316(4) 0.1800(4) -0.0123(2) 0.0288(10) Uani 1 1 d . . .
C32 C 0.6938(4) 0.1220(4) -0.0762(2) 0.0335(10) Uani 1 1 d . . .
H32 H 0.7834 0.1038 -0.0906 0.040 Uiso 1 1 calc R . .
C33 C 0.6246(5) 0.0904(4) -0.1192(3) 0.0405(12) Uani 1 1 d . . .
H33 H 0.6673 0.0515 -0.1631 0.049 Uiso 1 1 calc R . .
C34 C 0.4958(5) 0.1150(5) -0.0985(3) 0.0421(12) Uani 1 1 d . . .
H34 H 0.4494 0.0920 -0.1277 0.051 Uiso 1 1 calc R . .
C35 C 0.4328(5) 0.1731(5) -0.0352(3) 0.0508(14) Uani 1 1 d . . .
H35 H 0.3431 0.1918 -0.0216 0.061 Uiso 1 1 calc R . .
C36 C 0.5005(5) 0.2045(5) 0.0088(3) 0.0429(12) Uani 1 1 d . . .
H36 H 0.4573 0.2423 0.0531 0.051 Uiso 1 1 calc R . .
C37 C 0.7505(4) 0.3639(4) 0.0129(2) 0.0326(10) Uani 1 1 d . . .
C38 C 0.7955(5) 0.4215(4) 0.0567(3) 0.0430(12) Uani 1 1 d . . .
H38 H 0.7977 0.3887 0.1063 0.052 Uiso 1 1 calc R . .
C39 C 0.8371(5) 0.5265(5) 0.0282(4) 0.0613(17) Uani 1 1 d . . .
H39 H 0.8663 0.5667 0.0587 0.074 Uiso 1 1 calc R . .
C40 C 0.8365(6) 0.5734(5) -0.0438(4) 0.0641(17) Uani 1 1 d . . .
H40 H 0.8668 0.6448 -0.0632 0.077 Uiso 1 1 calc R . .
C41 C 0.7922(6) 0.5171(5) -0.0877(3) 0.0679(18) Uani 1 1 d . . .
H41 H 0.7912 0.5502 -0.1374 0.081 Uiso 1 1 calc R . .
C42 C 0.7491(5) 0.4128(5) -0.0600(3) 0.0497(14) Uani 1 1 d . . .
H42 H 0.7184 0.3742 -0.0906 0.060 Uiso 1 1 calc R . .
C43 C 0.1305(10) 0.8396(7) 0.4403(5) 0.133(3) Uani 1 1 d U . .
H43A H 0.1785 0.8880 0.4555 0.199 Uiso 1 1 calc R . .
H43B H 0.0400 0.8725 0.4595 0.199 Uiso 1 1 calc R . .
H43C H 0.1485 0.8443 0.3861 0.199 Uiso 1 1 calc R . .
C44 C 0.1659(5) 0.7158(4) 0.4692(3) 0.0844(19) Uani 1 1 d GU . .
C45 C 0.0762(4) 0.6543(5) 0.5109(3) 0.089(2) Uani 1 1 d GU . .
H45 H -0.0108 0.6953 0.5204 0.106 Uiso 1 1 calc R . .
C46 C 0.1139(6) 0.5326(5) 0.5387(3) 0.121(3) Uani 1 1 d GU . .
H46 H 0.0526 0.4905 0.5672 0.145 Uiso 1 1 calc R . .
C47 C 0.2412(7) 0.4725(4) 0.5248(3) 0.122(3) Uani 1 1 d GU . .
H47 H 0.2669 0.3894 0.5438 0.147 Uiso 1 1 calc R . .
C48 C 0.3309(5) 0.5341(5) 0.4831(4) 0.129(3) Uani 1 1 d GU . .
H48 H 0.4180 0.4930 0.4736 0.155 Uiso 1 1 calc R . .
C49 C 0.2933(5) 0.6557(5) 0.4553(3) 0.106(3) Uani 1 1 d GU . .
H49 H 0.3546 0.6978 0.4268 0.127 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0238(3) 0.0299(3) 0.0198(3) -0.0013(2) -0.0061(2) -0.0063(2)
N1 0.030(2) 0.032(2) 0.0159(18) -0.0026(15) -0.0098(15) -0.0042(16)
N2 0.0244(19) 0.0246(18) 0.026(2) -0.0021(15) -0.0136(15) -0.0047(15)
O1 0.0250(16) 0.0341(16) 0.0221(15) -0.0078(12) -0.0103(12) -0.0051(13)
O2 0.0250(16) 0.0347(17) 0.0225(16) -0.0012(13) -0.0085(12) -0.0027(13)
P1 0.0231(6) 0.0333(6) 0.0187(6) -0.0019(5) -0.0066(5) -0.0041(5)
P2 0.0287(6) 0.0271(6) 0.0196(6) -0.0019(5) -0.0076(5) -0.0055(5)
C1 0.024(2) 0.045(3) 0.021(2) -0.0021(19) -0.0073(18) -0.010(2)
C2 0.027(2) 0.037(2) 0.012(2) -0.0051(17) -0.0063(17) -0.0142(19)
C3 0.041(3) 0.033(2) 0.019(2) -0.0006(18) -0.013(2) -0.013(2)
C4 0.057(3) 0.040(3) 0.024(2) -0.001(2) -0.018(2) -0.018(3)
C5 0.036(3) 0.055(3) 0.022(2) -0.001(2) -0.011(2) -0.022(2)
C6 0.050(3) 0.031(3) 0.029(3) -0.002(2) -0.013(2) -0.003(2)
C7 0.059(4) 0.051(3) 0.043(3) -0.001(3) -0.004(3) 0.001(3)
C8 0.053(4) 0.062(4) 0.085(5) -0.030(3) -0.037(3) 0.016(3)
C9 0.083(4) 0.026(3) 0.072(4) 0.005(3) -0.001(3) -0.005(3)
C10 0.027(2) 0.036(2) 0.020(2) -0.0044(19) -0.0078(18) -0.0038(19)
C11 0.035(3) 0.038(3) 0.052(3) 0.009(2) -0.010(2) -0.007(2)
C12 0.057(4) 0.043(3) 0.052(3) 0.014(3) -0.021(3) -0.016(3)
C13 0.063(4) 0.042(3) 0.048(3) 0.000(3) -0.015(3) 0.003(3)
C14 0.051(3) 0.059(4) 0.043(3) 0.008(3) -0.004(3) 0.015(3)
C15 0.039(3) 0.052(3) 0.036(3) 0.016(2) -0.005(2) 0.003(2)
C16 0.029(2) 0.030(2) 0.020(2) -0.0046(18) -0.0078(19) -0.0003(19)
C17 0.046(3) 0.037(3) 0.031(3) 0.000(2) -0.012(2) -0.010(2)
C18 0.064(4) 0.049(3) 0.024(3) -0.004(2) -0.019(2) -0.004(3)
C19 0.067(4) 0.046(3) 0.017(2) -0.002(2) -0.003(2) -0.010(3)
C20 0.050(3) 0.056(3) 0.029(3) 0.001(2) 0.002(2) -0.016(3)
C21 0.037(3) 0.051(3) 0.023(2) 0.002(2) -0.007(2) -0.016(2)
C22 0.030(2) 0.026(2) 0.018(2) -0.0042(17) -0.0047(18) -0.0072(18)
C23 0.022(2) 0.025(2) 0.022(2) -0.0053(17) -0.0048(18) 0.0003(17)
C24 0.027(2) 0.028(2) 0.024(2) -0.0020(18) -0.0075(19) -0.0047(18)
C25 0.018(2) 0.035(3) 0.035(3) -0.001(2) -0.0074(19) -0.0085(19)
C26 0.029(2) 0.032(2) 0.023(2) -0.0063(19) 0.0017(19) -0.0100(19)
C27 0.024(2) 0.033(2) 0.031(3) -0.0059(19) -0.0080(19) -0.0104(19)
C28 0.039(3) 0.047(3) 0.035(3) -0.017(2) -0.012(2) -0.005(2)
C29 0.034(3) 0.050(3) 0.024(2) 0.000(2) -0.011(2) -0.011(2)
C30 0.038(3) 0.068(4) 0.034(3) -0.009(3) -0.013(2) -0.013(3)
C31 0.034(3) 0.026(2) 0.026(2) 0.0006(18) -0.012(2) -0.0036(19)
C32 0.034(3) 0.033(2) 0.032(3) -0.005(2) -0.012(2) 0.000(2)
C33 0.051(3) 0.046(3) 0.031(3) -0.009(2) -0.020(2) -0.009(2)
C34 0.048(3) 0.052(3) 0.036(3) -0.005(2) -0.023(2) -0.014(3)
C35 0.034(3) 0.077(4) 0.051(4) -0.009(3) -0.018(3) -0.020(3)
C36 0.039(3) 0.056(3) 0.038(3) -0.014(2) -0.015(2) -0.007(2)
C37 0.035(3) 0.030(2) 0.032(3) -0.004(2) -0.007(2) -0.005(2)
C38 0.054(3) 0.037(3) 0.043(3) -0.002(2) -0.014(3) -0.017(2)
C39 0.066(4) 0.042(3) 0.085(5) -0.017(3) -0.015(3) -0.024(3)
C40 0.082(5) 0.037(3) 0.073(5) 0.006(3) -0.012(4) -0.025(3)
C41 0.111(5) 0.039(3) 0.054(4) 0.019(3) -0.025(4) -0.024(3)
C42 0.076(4) 0.038(3) 0.038(3) 0.006(2) -0.016(3) -0.021(3)
C43 0.208(10) 0.079(5) 0.090(7) -0.010(5) -0.031(6) 0.000(5)
C44 0.107(5) 0.080(4) 0.072(5) -0.011(4) -0.031(4) -0.021(4)
C45 0.111(5) 0.116(5) 0.047(4) -0.032(4) 0.016(4) -0.058(4)
C46 0.166(7) 0.116(6) 0.079(6) -0.038(5) 0.010(6) -0.046(6)
C47 0.192(9) 0.095(6) 0.081(6) -0.018(5) -0.035(6) -0.027(5)
C48 0.125(7) 0.110(6) 0.177(10) -0.024(6) -0.077(6) -0.023(5)
C49 0.074(4) 0.113(6) 0.143(8) -0.003(5) -0.046(5) -0.027(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 1.918(3) . ?
Zn1 N1 1.953(3) . ?
Zn1 O1 2.017(3) . ?
Zn1 O2 2.062(3) . ?
N1 C2 1.387(5) . ?
N1 C3 1.390(5) . ?
N2 C24 1.375(5) . ?
N2 C23 1.418(5) . ?
O1 P1 1.497(3) . ?
O2 P2 1.500(3) . ?
P1 C1 1.799(4) . ?
P1 C16 1.801(4) . ?
P1 C10 1.803(4) . ?
P2 C37 1.786(4) . ?
P2 C31 1.790(4) . ?
P2 C22 1.800(4) . ?
C1 C2 1.503(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.366(6) . ?
C3 C4 1.382(6) . ?
C3 C6 1.500(6) . ?
C4 C5 1.395(7) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C8 1.522(7) . ?
C6 C9 1.542(6) . ?
C6 C7 1.557(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.381(6) . ?
C10 C15 1.384(6) . ?
C11 C12 1.387(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.388(6) . ?
C16 C21 1.389(6) . ?
C17 C18 1.394(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.370(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.368(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.393(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.499(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C26 1.356(5) . ?
C24 C25 1.385(5) . ?
C24 C27 1.529(6) . ?
C25 C26 1.407(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C30 1.515(6) . ?
C27 C29 1.525(6) . ?
C27 C28 1.537(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.388(6) . ?
C31 C36 1.391(6) . ?
C32 C33 1.394(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.366(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.383(6) . ?
C37 C42 1.394(6) . ?
C38 C39 1.380(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.371(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.370(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.378(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.414(8) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.3900 . ?
C44 C49 1.3900 . ?
C45 C46 1.3900 . ?
C45 H45 0.9500 . ?
C46 C47 1.3900 . ?
C46 H46 0.9500 . ?
C47 C48 1.3900 . ?
C47 H47 0.9500 . ?
C48 C49 1.3900 . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zn1 N1 136.21(14) . . ?
N2 Zn1 O1 115.17(12) . . ?
N1 Zn1 O1 99.75(12) . . ?
N2 Zn1 O2 96.97(12) . . ?
N1 Zn1 O2 106.67(12) . . ?
O1 Zn1 O2 93.72(11) . . ?
C2 N1 C3 106.2(3) . . ?
C2 N1 Zn1 116.2(3) . . ?
C3 N1 Zn1 137.2(3) . . ?
C24 N2 C23 105.5(3) . . ?
C24 N2 Zn1 135.2(3) . . ?
C23 N2 Zn1 119.3(2) . . ?
P1 O1 Zn1 118.37(15) . . ?
P2 O2 Zn1 120.17(16) . . ?
O1 P1 C1 110.28(17) . . ?
O1 P1 C16 110.20(18) . . ?
C1 P1 C16 109.03(19) . . ?
O1 P1 C10 109.54(18) . . ?
C1 P1 C10 108.86(19) . . ?
C16 P1 C10 108.89(19) . . ?
O2 P2 C37 112.23(19) . . ?
O2 P2 C31 110.64(18) . . ?
C37 P2 C31 109.4(2) . . ?
O2 P2 C22 109.72(17) . . ?
C37 P2 C22 106.6(2) . . ?
C31 P2 C22 108.14(19) . . ?
C2 C1 P1 112.8(3) . . ?
C2 C1 H1A 109.0 . . ?
P1 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
P1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C5 C2 N1 110.1(4) . . ?
C5 C2 C1 128.4(4) . . ?
N1 C2 C1 121.5(3) . . ?
C4 C3 N1 108.9(4) . . ?
C4 C3 C6 127.1(4) . . ?
N1 C3 C6 124.1(4) . . ?
C3 C4 C5 107.7(4) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
C2 C5 C4 107.2(4) . . ?
C2 C5 H5 126.4 . . ?
C4 C5 H5 126.4 . . ?
C3 C6 C8 112.8(4) . . ?
C3 C6 C9 111.0(4) . . ?
C8 C6 C9 108.1(4) . . ?
C3 C6 C7 110.3(4) . . ?
C8 C6 C7 107.7(4) . . ?
C9 C6 C7 106.9(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 119.0(4) . . ?
C11 C10 P1 118.3(3) . . ?
C15 C10 P1 122.7(3) . . ?
C10 C11 C12 120.6(5) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.5(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 120.6(5) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C15 119.8(5) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C10 120.6(5) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
C17 C16 C21 120.0(4) . . ?
C17 C16 P1 117.0(3) . . ?
C21 C16 P1 122.9(3) . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.1(5) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.8(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C20 119.2(4) . . ?
C16 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 P2 113.6(3) . . ?
C23 C22 H22A 108.8 . . ?
P2 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
P2 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C26 C23 N2 110.2(3) . . ?
C26 C23 C22 129.0(4) . . ?
N2 C23 C22 120.8(3) . . ?
N2 C24 C25 109.6(4) . . ?
N2 C24 C27 122.7(4) . . ?
C25 C24 C27 127.1(4) . . ?
C24 C25 C26 107.7(4) . . ?
C24 C25 H25 126.1 . . ?
C26 C25 H25 126.1 . . ?
C23 C26 C25 107.0(4) . . ?
C23 C26 H26 126.5 . . ?
C25 C26 H26 126.5 . . ?
C30 C27 C29 108.2(4) . . ?
C30 C27 C24 110.4(3) . . ?
C29 C27 C24 112.8(3) . . ?
C30 C27 C28 107.7(4) . . ?
C29 C27 C28 109.0(4) . . ?
C24 C27 C28 108.6(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 119.5(4) . . ?
C32 C31 P2 122.6(3) . . ?
C36 C31 P2 117.8(3) . . ?
C31 C32 C33 119.9(4) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.5(5) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 120.2(5) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 119.8(5) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C38 C37 C42 119.1(4) . . ?
C38 C37 P2 119.1(4) . . ?
C42 C37 P2 121.4(3) . . ?
C39 C38 C37 120.0(5) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C40 C39 C38 120.6(5) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C41 C40 C39 120.0(5) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.2(6) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C41 C42 C37 120.2(5) . . ?
C41 C42 H42 119.9 . . ?
C37 C42 H42 119.9 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C49 120.0 . . ?
C45 C44 C43 121.3(6) . . ?
C49 C44 C43 118.7(6) . . ?
C46 C45 C44 120.0 . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C47 C46 C45 120.0 . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C47 C48 120.0 . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 C49 120.0 . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 C44 120.0 . . ?
C48 C49 H49 120.0 . . ?
C44 C49 H49 120.0 . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 27.70
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 1.227
_refine_diff_density_min -0.826
_refine_diff_density_rms 0.121
#==END
data_8a
_database_code_depnum_ccdc_archive 'CCDC 729822'
_chemical_name_common 'Compound 8a'
_chemical_melting_point ?
_chemical_formula_structural '[Pyr-P(O)Ph2]3Y.PhMe'
_chemical_formula_moiety 'C51 H45 N3 O3 P3 Y, C7 H8'
_chemical_formula_sum 'C58 H53 N3 O3 P3 Y'
_chemical_formula_weight 1021.85
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 14.899(3)
_cell_length_b 18.890(3)
_cell_length_c 22.165(3)
_cell_angle_alpha 90.00
_cell_angle_beta 127.768(10)
_cell_angle_gamma 90.00
_cell_volume 4931.2(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 140(2)
_cell_measurement_reflns_used 1368
_cell_measurement_theta_min 3.4279
_cell_measurement_theta_max 27.5
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.376
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2120
_exptl_absorpt_coefficient_mu 1.329
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_absorpt_correction_T_min 0.7845
_exptl_absorpt_correction_T_max 0.9498
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 140(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_detector_area_resol_mean 16.005
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method 'Thin slice \f and \w scans'
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 40276
_diffrn_reflns_av_R_equivalents 0.3797
_diffrn_reflns_av_sigmaI/netI 0.4040
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 3.44
_diffrn_reflns_theta_max 22.50
_reflns_number_total 6410
_reflns_number_gt 1968
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Crystals of 8a were weakly diffracting, and this limited the maximum
2theta value to 45.0 degrees.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6410
_refine_ls_number_parameters 495
_refine_ls_number_restraints 622
_refine_ls_R_factor_all 0.2801
_refine_ls_R_factor_gt 0.0892
_refine_ls_wR_factor_ref 0.1817
_refine_ls_wR_factor_gt 0.1283
_refine_ls_goodness_of_fit_ref 0.857
_refine_ls_restrained_S_all 0.835
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.18353(14) 0.29524(7) 0.04072(9) 0.0302(4) Uani 1 1 d U . .
P1 P -0.0059(3) 0.35015(19) 0.0730(2) 0.0287(11) Uani 1 1 d U . .
P2 P 0.0312(4) 0.1430(2) -0.0355(2) 0.0365(11) Uani 1 1 d U . .
P3 P 0.3589(4) 0.3611(2) 0.0016(2) 0.0404(12) Uani 1 1 d U . .
O1 O 0.0374(6) 0.2956(4) 0.0471(4) 0.0254(19) Uani 1 1 d U . .
O2 O 0.0737(7) 0.2104(5) -0.0464(4) 0.035(2) Uani 1 1 d U . .
O3 O 0.3284(7) 0.3080(5) 0.0362(5) 0.038(2) Uani 1 1 d U . .
N1 N 0.2511(10) 0.3796(5) 0.1366(6) 0.033(3) Uani 1 1 d U . .
N2 N 0.2753(10) 0.1923(6) 0.1141(6) 0.038(3) Uani 1 1 d U . .
N3 N 0.0993(10) 0.3792(5) -0.0589(6) 0.026(3) Uani 1 1 d U . .
C1 C 0.0672(11) 0.4311(6) 0.0938(7) 0.031(3) Uani 1 1 d U . .
H1A H 0.0501 0.4507 0.0463 0.038 Uiso 1 1 calc R . .
H1B H 0.0400 0.4654 0.1131 0.038 Uiso 1 1 calc R . .
C2 C 0.1937(13) 0.4221(6) 0.1522(8) 0.027(3) Uani 1 1 d U . .
C3 C 0.3622(13) 0.3849(7) 0.1990(8) 0.042(4) Uani 1 1 d U . .
H3 H 0.4229 0.3616 0.2039 0.050 Uiso 1 1 calc R . .
C4 C 0.3764(14) 0.4294(7) 0.2557(9) 0.046(4) Uani 1 1 d U . .
H4 H 0.4446 0.4417 0.3041 0.055 Uiso 1 1 calc R . .
C5 C 0.2651(13) 0.4509(7) 0.2228(8) 0.043(4) Uani 1 1 d U . .
H5 H 0.2432 0.4807 0.2463 0.052 Uiso 1 1 calc R . .
C6 C -0.1534(6) 0.3654(5) -0.0006(4) 0.024(3) Uani 1 1 d GU . .
C7 C -0.1894(8) 0.4187(4) -0.0542(5) 0.039(4) Uani 1 1 d GU . .
H7 H -0.1353 0.4492 -0.0503 0.046 Uiso 1 1 calc R . .
C8 C -0.3044(9) 0.4275(4) -0.1134(5) 0.051(4) Uani 1 1 d GU . .
H8 H -0.3290 0.4639 -0.1500 0.061 Uiso 1 1 calc R . .
C9 C -0.3835(6) 0.3829(6) -0.1190(5) 0.063(5) Uani 1 1 d GU . .
H9 H -0.4621 0.3889 -0.1594 0.075 Uiso 1 1 calc R . .
C10 C -0.3475(8) 0.3295(5) -0.0654(6) 0.088(6) Uani 1 1 d GU . .
H10 H -0.4015 0.2991 -0.0693 0.105 Uiso 1 1 calc R . .
C11 C -0.2324(9) 0.3208(4) -0.0062(5) 0.073(5) Uani 1 1 d GU . .
H11 H -0.2078 0.2843 0.0304 0.088 Uiso 1 1 calc R . .
C12 C 0.0095(7) 0.3203(4) 0.1551(4) 0.022(3) Uani 1 1 d GU . .
C13 C 0.0099(7) 0.2482(4) 0.1679(4) 0.030(4) Uani 1 1 d GU . .
H13 H 0.0034 0.2149 0.1333 0.036 Uiso 1 1 calc R . .
C14 C 0.0200(8) 0.2249(3) 0.2312(5) 0.037(4) Uani 1 1 d GU . .
H14 H 0.0203 0.1756 0.2399 0.044 Uiso 1 1 calc R . .
C15 C 0.0296(7) 0.2736(5) 0.2819(4) 0.034(4) Uani 1 1 d GU . .
H15 H 0.0365 0.2577 0.3252 0.040 Uiso 1 1 calc R . .
C16 C 0.0292(8) 0.3457(4) 0.2692(4) 0.045(4) Uani 1 1 d GU . .
H16 H 0.0358 0.3791 0.3038 0.054 Uiso 1 1 calc R . .
C17 C 0.0191(8) 0.3691(3) 0.2058(5) 0.038(4) Uani 1 1 d GU . .
H17 H 0.0188 0.4183 0.1971 0.046 Uiso 1 1 calc R . .
C18 C 0.1001(12) 0.1254(7) 0.0639(7) 0.039(3) Uani 1 1 d U . .
H18A H 0.0742 0.1602 0.0837 0.046 Uiso 1 1 calc R . .
H18B H 0.0787 0.0776 0.0694 0.046 Uiso 1 1 calc R . .
C19 C 0.2265(13) 0.1298(8) 0.1095(8) 0.037(3) Uani 1 1 d U . .
C20 C 0.3837(14) 0.1761(8) 0.1558(8) 0.055(4) Uani 1 1 d U . .
H20 H 0.4405 0.2097 0.1691 0.066 Uiso 1 1 calc R . .
C21 C 0.4077(15) 0.1078(8) 0.1781(8) 0.054(4) Uani 1 1 d U . .
H21 H 0.4803 0.0858 0.2078 0.065 Uiso 1 1 calc R . .
C22 C 0.3040(15) 0.0764(8) 0.1485(8) 0.052(4) Uani 1 1 d U . .
H22 H 0.2899 0.0287 0.1539 0.063 Uiso 1 1 calc R . .
C23 C 0.0564(8) 0.0700(4) -0.0742(5) 0.028(3) Uani 1 1 d GU . .
C24 C 0.1671(7) 0.0600(4) -0.0485(4) 0.032(3) Uani 1 1 d GU . .
H24 H 0.2254 0.0916 -0.0121 0.038 Uiso 1 1 calc R . .
C25 C 0.1928(6) 0.0036(5) -0.0759(5) 0.042(4) Uani 1 1 d GU . .
H25 H 0.2685 -0.0032 -0.0583 0.050 Uiso 1 1 calc R . .
C26 C 0.1076(9) -0.0426(4) -0.1291(5) 0.049(4) Uani 1 1 d GU . .
H26 H 0.1251 -0.0811 -0.1479 0.058 Uiso 1 1 calc R . .
C27 C -0.0032(8) -0.0326(4) -0.1549(4) 0.043(4) Uani 1 1 d GU . .
H27 H -0.0614 -0.0642 -0.1913 0.052 Uiso 1 1 calc R . .
C28 C -0.0288(6) 0.0238(5) -0.1275(5) 0.036(4) Uani 1 1 d GU . .
H28 H -0.1046 0.0307 -0.1451 0.044 Uiso 1 1 calc R . .
C29 C -0.1183(7) 0.1478(5) -0.0827(5) 0.043(3) Uani 1 1 d GU . .
C30 C -0.1828(9) 0.2003(5) -0.1367(6) 0.083(6) Uani 1 1 d GU . .
H30 H -0.1487 0.2314 -0.1512 0.100 Uiso 1 1 calc R . .
C31 C -0.2972(9) 0.2075(5) -0.1696(5) 0.103(7) Uani 1 1 d GU . .
H31 H -0.3413 0.2434 -0.2065 0.123 Uiso 1 1 calc R . .
C32 C -0.3470(6) 0.1621(6) -0.1485(6) 0.082(6) Uani 1 1 d GU . .
H32 H -0.4252 0.1670 -0.1710 0.099 Uiso 1 1 calc R . .
C33 C -0.2825(9) 0.1096(5) -0.0945(6) 0.058(4) Uani 1 1 d GU . .
H33 H -0.3166 0.0785 -0.0801 0.070 Uiso 1 1 calc R . .
C34 C -0.1681(9) 0.1024(4) -0.0616(5) 0.059(4) Uani 1 1 d GU . .
H34 H -0.1240 0.0665 -0.0247 0.071 Uiso 1 1 calc R . .
C35 C 0.2754(11) 0.4369(7) -0.0255(8) 0.043(4) Uani 1 1 d U . .
H35A H 0.2934 0.4598 0.0210 0.051 Uiso 1 1 calc R . .
H35B H 0.2962 0.4706 -0.0493 0.051 Uiso 1 1 calc R . .
C36 C 0.1481(13) 0.4239(7) -0.0807(9) 0.036(3) Uani 1 1 d U . .
C37 C -0.0106(12) 0.3773(6) -0.1209(8) 0.033(4) Uani 1 1 d U . .
H37 H -0.0669 0.3505 -0.1235 0.040 Uiso 1 1 calc R . .
C38 C -0.0323(13) 0.4171(6) -0.1784(8) 0.031(4) Uani 1 1 d U . .
H38 H -0.1044 0.4243 -0.2263 0.037 Uiso 1 1 calc R . .
C39 C 0.0711(12) 0.4461(7) -0.1548(8) 0.035(4) Uani 1 1 d U . .
H39 H 0.0848 0.4747 -0.1836 0.041 Uiso 1 1 calc R . .
C40 C 0.5030(8) 0.3880(5) 0.0700(5) 0.046(4) Uani 1 1 d GU . .
C41 C 0.5369(9) 0.4264(6) 0.1343(7) 0.077(5) Uani 1 1 d GU . .
H41 H 0.4822 0.4413 0.1406 0.093 Uiso 1 1 calc R . .
C42 C 0.6509(10) 0.4430(5) 0.1894(5) 0.088(6) Uani 1 1 d GU . .
H42 H 0.6741 0.4692 0.2333 0.105 Uiso 1 1 calc R . .
C43 C 0.7309(7) 0.4211(5) 0.1802(6) 0.076(5) Uani 1 1 d GU . .
H43 H 0.8088 0.4324 0.2178 0.091 Uiso 1 1 calc R . .
C44 C 0.6969(10) 0.3827(6) 0.1158(7) 0.103(6) Uani 1 1 d GU . .
H44 H 0.7516 0.3677 0.1095 0.124 Uiso 1 1 calc R . .
C45 C 0.5830(11) 0.3661(6) 0.0607(6) 0.098(5) Uani 1 1 d GU . .
H45 H 0.5598 0.3399 0.0168 0.118 Uiso 1 1 calc R . .
C46 C 0.3385(8) 0.3244(6) -0.0796(5) 0.039(4) Uani 1 1 d GU . .
C47 C 0.3355(8) 0.3676(5) -0.1316(6) 0.066(4) Uani 1 1 d GU . .
H47 H 0.3436 0.4174 -0.1241 0.079 Uiso 1 1 calc R . .
C48 C 0.3207(8) 0.3380(7) -0.1945(5) 0.077(5) Uani 1 1 d GU . .
H48 H 0.3186 0.3675 -0.2300 0.092 Uiso 1 1 calc R . .
C49 C 0.3089(9) 0.2651(7) -0.2055(5) 0.082(5) Uani 1 1 d GU . .
H49 H 0.2987 0.2448 -0.2485 0.098 Uiso 1 1 calc R . .
C50 C 0.3119(9) 0.2219(5) -0.1535(6) 0.075(5) Uani 1 1 d GU . .
H50 H 0.3038 0.1721 -0.1610 0.090 Uiso 1 1 calc R . .
C51 C 0.3267(8) 0.2516(5) -0.0905(5) 0.059(4) Uani 1 1 d GU . .
H51 H 0.3288 0.2221 -0.0550 0.071 Uiso 1 1 calc R . .
C101 C 0.6527(13) 0.1549(8) 1.1350(7) 0.157(9) Uiso 1 1 d GDU . .
C102 C 0.5601(13) 0.1093(7) 1.0966(10) 0.167(10) Uiso 1 1 d GDU . .
H102 H 0.5337 0.0893 1.1225 0.201 Uiso 1 1 calc R . .
C103 C 0.5061(11) 0.0929(7) 1.0204(10) 0.216(12) Uiso 1 1 d GU . .
H103 H 0.4429 0.0617 0.9942 0.260 Uiso 1 1 calc R . .
C104 C 0.5448(13) 0.1221(8) 0.9826(7) 0.139(8) Uiso 1 1 d GU . .
H104 H 0.5079 0.1110 0.9305 0.166 Uiso 1 1 calc R . .
C105 C 0.6373(14) 0.1678(7) 1.0209(9) 0.128(8) Uiso 1 1 d GU . .
H105 H 0.6638 0.1878 0.9950 0.154 Uiso 1 1 calc R . .
C106 C 0.6913(11) 0.1842(6) 1.0971(9) 0.175(10) Uiso 1 1 d GDU . .
H106 H 0.7546 0.2153 1.1233 0.209 Uiso 1 1 calc R . .
C107 C 0.695(3) 0.1849(15) 1.2080(10) 0.325(19) Uiso 1 1 d DU . .
H10A H 0.6562 0.2299 1.2000 0.487 Uiso 1 1 calc R . .
H10B H 0.7767 0.1931 1.2382 0.487 Uiso 1 1 calc R . .
H10C H 0.6803 0.1520 1.2352 0.487 Uiso 1 1 calc RD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.0346(10) 0.0398(9) 0.0262(9) -0.0045(9) 0.0237(8) -0.0042(10)
P1 0.037(3) 0.031(2) 0.027(3) 0.0071(19) 0.024(2) 0.004(2)
P2 0.045(3) 0.038(2) 0.031(3) 0.000(2) 0.026(2) -0.001(2)
P3 0.042(3) 0.043(3) 0.039(3) -0.002(2) 0.026(3) -0.006(2)
O1 0.025(5) 0.031(5) 0.025(5) 0.002(4) 0.017(4) 0.001(4)
O2 0.044(6) 0.036(4) 0.029(5) -0.005(4) 0.025(4) -0.007(5)
O3 0.029(5) 0.054(6) 0.033(6) 0.013(5) 0.019(5) 0.005(4)
N1 0.023(6) 0.041(7) 0.031(6) -0.008(5) 0.015(5) -0.007(5)
N2 0.034(6) 0.042(6) 0.035(6) 0.000(5) 0.019(5) 0.003(5)
N3 0.029(6) 0.026(6) 0.027(5) -0.004(4) 0.020(5) -0.008(5)
C1 0.032(6) 0.041(7) 0.023(8) 0.011(6) 0.018(6) 0.007(6)
C2 0.032(6) 0.013(8) 0.036(8) 0.001(6) 0.020(6) 0.003(6)
C3 0.022(7) 0.053(10) 0.044(9) -0.021(7) 0.017(7) -0.016(7)
C4 0.036(8) 0.059(10) 0.033(9) -0.017(7) 0.016(7) -0.012(8)
C5 0.040(8) 0.061(10) 0.024(8) -0.002(7) 0.017(7) 0.000(8)
C6 0.033(5) 0.025(7) 0.034(6) -0.001(5) 0.031(5) 0.004(5)
C7 0.034(7) 0.046(9) 0.034(10) 0.006(6) 0.020(7) -0.011(7)
C8 0.033(8) 0.087(11) 0.029(9) 0.012(8) 0.017(7) 0.002(8)
C9 0.025(9) 0.119(14) 0.027(10) 0.014(8) 0.008(8) -0.007(8)
C10 0.044(8) 0.148(15) 0.049(12) 0.029(9) 0.018(8) -0.030(10)
C11 0.047(7) 0.093(11) 0.060(10) 0.037(8) 0.023(7) -0.021(8)
C12 0.014(8) 0.023(7) 0.031(7) 0.000(5) 0.015(6) -0.006(6)
C13 0.046(10) 0.020(6) 0.040(9) 0.005(6) 0.034(8) -0.002(7)
C14 0.047(10) 0.035(8) 0.060(10) 0.011(6) 0.049(9) 0.002(7)
C15 0.026(8) 0.051(8) 0.032(8) 0.008(6) 0.022(8) 0.002(8)
C16 0.058(11) 0.049(7) 0.049(9) -0.004(7) 0.044(9) -0.007(9)
C17 0.059(11) 0.026(7) 0.039(9) 0.008(6) 0.034(9) 0.012(8)
C18 0.051(7) 0.041(9) 0.031(7) 0.000(6) 0.029(7) -0.010(7)
C19 0.053(6) 0.046(7) 0.027(7) 0.009(7) 0.033(6) 0.001(6)
C20 0.044(6) 0.066(7) 0.046(8) 0.010(6) 0.023(6) 0.008(5)
C21 0.062(8) 0.066(9) 0.042(11) 0.005(8) 0.036(9) 0.028(8)
C22 0.079(10) 0.051(8) 0.045(11) 0.009(8) 0.047(10) 0.016(7)
C23 0.034(6) 0.029(6) 0.016(6) 0.009(4) 0.012(5) 0.001(5)
C24 0.041(6) 0.043(7) 0.023(6) 0.001(5) 0.025(5) -0.002(5)
C25 0.046(9) 0.056(10) 0.020(9) 0.000(6) 0.018(8) 0.012(7)
C26 0.066(10) 0.047(9) 0.031(10) -0.001(6) 0.028(9) 0.006(8)
C27 0.062(9) 0.040(9) 0.027(9) 0.000(6) 0.027(9) -0.003(8)
C28 0.047(8) 0.039(9) 0.029(9) 0.002(6) 0.027(7) -0.014(6)
C29 0.044(6) 0.037(9) 0.049(9) -0.010(7) 0.029(6) -0.006(6)
C30 0.042(8) 0.082(12) 0.078(13) 0.032(8) 0.013(10) -0.007(9)
C31 0.041(9) 0.110(13) 0.092(13) 0.059(10) 0.007(10) -0.009(10)
C32 0.037(10) 0.091(14) 0.074(13) 0.017(8) 0.010(9) -0.018(8)
C33 0.060(10) 0.049(10) 0.085(13) 0.006(7) 0.055(11) -0.003(8)
C34 0.061(9) 0.040(9) 0.095(12) 0.001(8) 0.058(10) 0.002(8)
C35 0.033(6) 0.045(8) 0.060(10) 0.010(7) 0.034(7) -0.001(6)
C36 0.030(6) 0.050(9) 0.046(8) 0.001(6) 0.032(6) -0.003(6)
C37 0.033(7) 0.023(8) 0.039(8) -0.003(6) 0.020(6) -0.011(6)
C38 0.033(6) 0.025(7) 0.032(6) -0.008(5) 0.019(5) 0.009(5)
C39 0.044(8) 0.034(8) 0.050(8) 0.015(6) 0.041(6) 0.020(7)
C40 0.037(6) 0.071(11) 0.030(8) 0.002(6) 0.020(6) -0.002(6)
C41 0.051(9) 0.125(14) 0.063(12) -0.047(9) 0.038(9) -0.037(10)
C42 0.049(10) 0.127(14) 0.085(12) -0.053(10) 0.040(9) -0.042(11)
C43 0.048(10) 0.080(12) 0.092(11) -0.020(9) 0.039(9) -0.015(9)
C44 0.064(7) 0.122(10) 0.121(9) -0.038(7) 0.055(7) 0.003(7)
C45 0.064(6) 0.123(9) 0.100(9) -0.043(7) 0.046(6) 0.013(7)
C46 0.022(7) 0.057(7) 0.038(6) 0.000(5) 0.018(5) -0.004(6)
C47 0.040(10) 0.119(10) 0.055(10) 0.004(8) 0.038(10) -0.007(10)
C48 0.069(9) 0.125(8) 0.070(7) 0.007(6) 0.060(7) -0.005(7)
C49 0.062(9) 0.119(8) 0.074(8) 0.000(6) 0.046(7) 0.014(7)
C50 0.062(11) 0.098(10) 0.062(11) -0.026(8) 0.036(10) -0.005(10)
C51 0.046(11) 0.079(8) 0.052(10) -0.018(7) 0.031(10) 0.004(9)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O3 2.234(9) . ?
Y1 O2 2.259(8) . ?
Y1 O1 2.268(8) . ?
Y1 N1 2.334(10) . ?
Y1 N3 2.360(10) . ?
Y1 N2 2.361(11) . ?
P1 O1 1.503(8) . ?
P1 C1 1.767(12) . ?
P1 C12 1.782(7) . ?
P1 C6 1.783(8) . ?
P2 O2 1.507(9) . ?
P2 C23 1.781(7) . ?
P2 C29 1.790(8) . ?
P2 C18 1.802(12) . ?
P3 O3 1.493(9) . ?
P3 C35 1.746(13) . ?
P3 C46 1.771(8) . ?
P3 C40 1.782(9) . ?
N1 C3 1.364(15) . ?
N1 C2 1.364(16) . ?
N2 C20 1.315(16) . ?
N2 C19 1.358(15) . ?
N3 C37 1.348(15) . ?
N3 C36 1.380(16) . ?
C1 C2 1.506(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.354(16) . ?
C3 C4 1.414(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.402(19) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 C9 1.3900 . ?
C8 H8 0.9500 . ?
C9 C10 1.3900 . ?
C9 H9 0.9500 . ?
C10 C11 1.3900 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C12 C17 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 C17 1.3900 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.498(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C22 1.368(18) . ?
C20 C21 1.348(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(19) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 C27 1.3900 . ?
C26 H26 0.9500 . ?
C27 C28 1.3900 . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.3900 . ?
C29 C34 1.3900 . ?
C30 C31 1.3900 . ?
C30 H30 0.9500 . ?
C31 C32 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.520(17) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C39 1.372(16) . ?
C37 C38 1.338(16) . ?
C37 H37 0.9500 . ?
C38 C39 1.399(17) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.3900 . ?
C40 C45 1.3900 . ?
C41 C42 1.3900 . ?
C41 H41 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43 0.9500 . ?
C44 C45 1.3900 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.3900 . ?
C46 C51 1.3900 . ?
C47 C48 1.3900 . ?
C47 H47 0.9500 . ?
C48 C49 1.3900 . ?
C48 H48 0.9500 . ?
C49 C50 1.3900 . ?
C49 H49 0.9500 . ?
C50 C51 1.3900 . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C101 C107 1.445(10) . ?
C102 C103 1.3900 . ?
C102 H102 0.9500 . ?
C103 C104 1.3900 . ?
C103 H103 0.9500 . ?
C104 C105 1.3900 . ?
C104 H104 0.9500 . ?
C105 C106 1.3900 . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C107 H10A 0.9800 . ?
C107 H10B 0.9800 . ?
C107 H10C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Y1 O2 104.6(3) . . ?
O3 Y1 O1 173.6(3) . . ?
O2 Y1 O1 80.5(3) . . ?
O3 Y1 N1 94.4(4) . . ?
O2 Y1 N1 161.0(4) . . ?
O1 Y1 N1 80.6(4) . . ?
O3 Y1 N3 82.0(4) . . ?
O2 Y1 N3 89.1(3) . . ?
O1 Y1 N3 94.3(3) . . ?
N1 Y1 N3 94.5(3) . . ?
O3 Y1 N2 87.3(4) . . ?
O2 Y1 N2 79.4(3) . . ?
O1 Y1 N2 97.6(4) . . ?
N1 Y1 N2 100.9(4) . . ?
N3 Y1 N2 161.8(4) . . ?
O1 P1 C1 110.7(6) . . ?
O1 P1 C12 110.8(4) . . ?
C1 P1 C12 109.5(5) . . ?
O1 P1 C6 109.8(4) . . ?
C1 P1 C6 108.4(5) . . ?
C12 P1 C6 107.5(5) . . ?
O2 P2 C23 110.0(5) . . ?
O2 P2 C29 110.9(5) . . ?
C23 P2 C29 108.1(5) . . ?
O2 P2 C18 111.8(5) . . ?
C23 P2 C18 108.4(5) . . ?
C29 P2 C18 107.3(6) . . ?
O3 P3 C35 110.5(6) . . ?
O3 P3 C46 110.0(6) . . ?
C35 P3 C46 109.2(6) . . ?
O3 P3 C40 110.0(5) . . ?
C35 P3 C40 107.0(6) . . ?
C46 P3 C40 110.1(6) . . ?
P1 O1 Y1 132.7(5) . . ?
P2 O2 Y1 128.1(5) . . ?
P3 O3 Y1 134.6(5) . . ?
C3 N1 C2 105.0(12) . . ?
C3 N1 Y1 123.6(10) . . ?
C2 N1 Y1 130.2(10) . . ?
C20 N2 C19 102.7(13) . . ?
C20 N2 Y1 128.3(11) . . ?
C19 N2 Y1 127.4(10) . . ?
C37 N3 C36 103.3(12) . . ?
C37 N3 Y1 123.7(9) . . ?
C36 N3 Y1 130.3(10) . . ?
C2 C1 P1 112.0(9) . . ?
C2 C1 H1A 109.2 . . ?
P1 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
P1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C5 C2 N1 111.0(13) . . ?
C5 C2 C1 129.2(14) . . ?
N1 C2 C1 119.8(12) . . ?
N1 C3 C4 111.9(14) . . ?
N1 C3 H3 124.0 . . ?
C4 C3 H3 124.0 . . ?
C5 C4 C3 103.0(14) . . ?
C5 C4 H4 128.5 . . ?
C3 C4 H4 128.5 . . ?
C2 C5 C4 109.0(14) . . ?
C2 C5 H5 125.5 . . ?
C4 C5 H5 125.5 . . ?
C7 C6 C11 120.0 . . ?
C7 C6 P1 120.8(6) . . ?
C11 C6 P1 119.1(6) . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C6 120.0 . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
C13 C12 C17 120.0 . . ?
C13 C12 P1 119.9(5) . . ?
C17 C12 P1 120.1(5) . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C12 120.0 . . ?
C16 C17 H17 120.0 . . ?
C12 C17 H17 120.0 . . ?
C19 C18 P2 110.8(10) . . ?
C19 C18 H18A 109.5 . . ?
P2 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
P2 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N2 C19 C22 112.8(15) . . ?
N2 C19 C18 119.5(13) . . ?
C22 C19 C18 127.7(15) . . ?
N2 C20 C21 114.6(16) . . ?
N2 C20 H20 122.7 . . ?
C21 C20 H20 122.7 . . ?
C20 C21 C22 105.4(16) . . ?
C20 C21 H21 127.3 . . ?
C22 C21 H21 127.3 . . ?
C19 C22 C21 104.4(15) . . ?
C19 C22 H22 127.8 . . ?
C21 C22 H22 127.8 . . ?
C24 C23 C28 120.0 . . ?
C24 C23 P2 117.1(6) . . ?
C28 C23 P2 122.9(6) . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C23 120.0 . . ?
C27 C28 H28 120.0 . . ?
C23 C28 H28 120.0 . . ?
C30 C29 C34 120.0 . . ?
C30 C29 P2 119.8(7) . . ?
C34 C29 P2 120.1(7) . . ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 120.0 . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
C36 C35 P3 114.7(10) . . ?
C36 C35 H35A 108.6 . . ?
P3 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
P3 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C39 C36 N3 111.9(13) . . ?
C39 C36 C35 129.1(14) . . ?
N3 C36 C35 118.8(13) . . ?
C38 C37 N3 113.0(14) . . ?
C38 C37 H37 123.5 . . ?
N3 C37 H37 123.5 . . ?
C37 C38 C39 107.2(14) . . ?
C37 C38 H38 126.4 . . ?
C39 C38 H38 126.4 . . ?
C36 C39 C38 104.5(13) . . ?
C36 C39 H39 127.7 . . ?
C38 C39 H39 127.7 . . ?
C41 C40 C45 120.0 . . ?
C41 C40 P3 120.9(8) . . ?
C45 C40 P3 119.0(7) . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C45 C44 C43 120.0 . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C40 120.0 . . ?
C44 C45 H45 120.0 . . ?
C40 C45 H45 120.0 . . ?
C47 C46 C51 120.0 . . ?
C47 C46 P3 120.7(7) . . ?
C51 C46 P3 119.3(7) . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C47 C48 C49 120.0 . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C50 C49 C48 120.0 . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C51 C50 C49 120.0 . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C50 C51 C46 120.0 . . ?
C50 C51 H51 120.0 . . ?
C46 C51 H51 120.0 . . ?
C102 C101 C106 120.0 . . ?
C102 C101 C107 121.1(8) . . ?
C106 C101 C107 117.6(7) . . ?
C103 C102 C101 120.0 . . ?
C103 C102 H102 120.0 . . ?
C101 C102 H102 120.0 . . ?
C102 C103 C104 120.0 . . ?
C102 C103 H103 120.0 . . ?
C104 C103 H103 120.0 . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C103 C104 H104 120.0 . . ?
C106 C105 C104 120.0 . . ?
C106 C105 H105 120.0 . . ?
C104 C105 H105 120.0 . . ?
C105 C106 C101 120.0 . . ?
C105 C106 H106 120.0 . . ?
C101 C106 H106 120.0 . . ?
C101 C107 H10A 109.5 . . ?
C101 C107 H10B 109.5 . . ?
H10A C107 H10B 109.5 . . ?
C101 C107 H10C 109.5 . . ?
H10A C107 H10C 109.5 . . ?
H10B C107 H10C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 22.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.597
_refine_diff_density_min -0.530
_refine_diff_density_rms 0.083
#==END